phenylacetic acid from phenylalanine This search engine indexes the Drug Enforcement Administration Diversion Control Program Web Site (www.deadiversion.usdoj.gov) only. 60g of mercuric chloride contains 45 grams of Davies and Waring52 found that, if comparable quantities of phenylacetic acid and lead(IV)acetate are reacted, the major radical formed is a methyl radical, leading to benzyl acetate (26). Aside from the often amateurish reduction of (pseudo)ephedrine to methamphetamine, the most popular precursor to amphetamine and methamphetamine is How is mandelic acid produced? Methoxyphenylacetic acid is a natural product found in Olea europaea with data available. P2P can be manufactured by distilling phenylacetic acid using lead acetate as a reagent, or alternatively from benzene and chloroacetone using aluminum chloride as a reagent. Urinary phenylacetic acid (PAA) is the product of unidentified, specific strains of bacteria, marking a state of bacterial overgrowth when it is elevated in urine. A monocarboxylic acid that is toluene in which one of the hydrogens of the methyl group has been replaced by a carboxy group. with sulfuric acid, as it is much cheaper to use, and is not disastrous for your health or the environment. Clandestine Methamphetamine Manufacturing: (PDF 34 pages): (1938) A preparation of phenylacetone (PDF 45 pages): Secrets Of Methamphetamine Manufacture ( 5th Edition) Uncle Fester: Poor Bastards Guide To Making Amphetamine / Phenylacetone: (2005 Bulletin) Analyses of samples of 1-phenyl-2-propanone (PDF 30 pages): How Mexico Became the US's Main Meth Supplier: https://www.caymanchem.com/msdss/16103m.pdf, https://www.quora.com/What-is-the-chemical-P2P-and-what-is-its-original-design-intended-for, https://www.sog.unc.edu/sites/www.sog.unc.edu/files/course_materials/UNC_Meth_Presentation_29Oct2015_0.pdf, https://core.ac.uk/download/pdf/142068835.pdf, https://archive.org/details/secrets-of-methamphetamine-manufacture-5th-edition-uncle-fester/mode/2up, https://www.thevespiary.org/rhodium/Rhodium/Vespiary/talk/index.php/topic%2C800.0.html, https://www.thevespiary.org/rhodium/Rhodium/Vespiary/talk/index.php/topic%2c225.0.html, https://www.designer-drug.com/pte/12.162.180.114/dcd/chemistry/phenylacetone.html, http://www.sciencemadness.org/talk/viewthread.php?tid=80128, https://www.unodc.org/pdf/research/Bulletin07/Bulletin_on_narcotics_2007_Krawczyk.pdf, https://www.talkingdrugs.org/sites/default/files/images/meth-graph.JPG, https://www.reddit.com/search/?q=Phenylacetone, https://en.wikipedia.org/wiki/Phenylacetone, https://pubchem.ncbi.nlm.nih.gov/compound/Phenylacetone. These keto-alcohols undergo esterification, followed by elimination of acetic acid (Fig. Many of the syntheses of P2P described in the literature are outlined in Table 12-41. More. The oil and alpha-Methylstyrene can also be treated with Bromine and Sulfuric Acid to yield P2P. I made phenylacetone twice. The ketone was frozen Phenylacetic acid - Wikipedia ambient temperature (10-15 min), the yellow solution was diluted with water (150 mL), neutralized with powdered NaHCO3 and saturated with NaCl. The crude oil was purified by silica gel chromatography. This is the dimethyl cadmium, keep it 26, 3777 (1985) The reaction is initiated from the activated methylene compound, which condenses with the carbonyl of P2P. The solution of the grignard reagent was diluted with ether so that the concentration was no greater than 0.2 The mixture was stirred and heated to refluxing on a bicarb untill fizzing stops. Such strong bases include sodium amide, lithium diisopropylamide and several alkoxides, for example potassium tert-butoxide. hemihydrate (125g, 834 mmol; Aldrich). By analogy with NAD+-specific isocitrate and malate dehydrogenases, phenylmalonic semialdehyde, a 3-oxoacid, would be expected to be the precursor of phenylacetaldehyde. An organic extraction allowed clean isolation of all nonketonic compounds into an organic phase. The sodium salt is Another method for reducing phenyl-2-nitropropene to phenyl-2-propanone in 80% yield is to use Chromium(II)chloride as the There are other ways of performing this rearrangement, 2-phenylpropanal is isomerized to phenyl-2-propanone in up to 87% yield by passing its vapor over DO NOT ADD MORE!! Boiling point 92-94C/12mmHg, 222C/760mmHg. This salt is slightly hygroscopic on exposure in air but can be stored would be higher if reaction mixture was first poured onto ice, then acidified.] [13] Alexander Shulgin, Pihkal #109 Anhydrous cadmium chloride (0.16 mol) was added with vigorous stirring over 10-15 min. (Phenylacetic acid/AA/NaAc) High Bees! After the lithium metal was consumed completely, the stirring was stopped; metallic nickel which had adhered to the walls of the flask was scraped off with the stirrer and a magnet. sodium sulfate is collected on a filter, washed with ether, and discarded. Phenyl-2-Nitropropene (10 g, 61 mmol) was dissolved in 75 ml HOAc and slowly dripped into a refluxing slurry of Fe powder (32 g, 0.57 mol) in 140 ml corresponds 250-275g of dry sodium salt, or 69-76% of the calculated mount. 60, 5275-5280 (1970), Journal of Organic Chemistry, Vol. 2, p 487-489 Many of the earliest routes to the compound has been more or less Coll. [8] R. Ballini, Synthesis 723-726 (1994)[9] J. Amer. The second step is a proton removal from the activated methylene compound (mixed anhydride) by a base (sodium acetate or pyridine). The benzene was distilled off, and the remaining viscous oil was distilled under reduced pressure. condenser, stirring during the addition. I attempted to prepare phenylacetone again using a novel synthesis that I devised. Methoxy(phenyl)acetic acid. beaker containing 100 ml. Seventeen runs were made in order to determine the optimum conditions for the reaction and the most efficient method of purification. What is phenylacetic acid? | Technology Trends objective in this investigation to establish criteria by which these two synthetic routes can be distinguished on the basis The multi-step variants, and from the very easy to the very complicated. Fractional distillation could theoretically be used to separate them, but the These results confirm that 1 is a synthetic marker compound for the phenylacetic acid and lead (II) acetate method. of dry colorless alpha-phenylacetoacetonitrile, mp 87-89C. Other condensations of activated methylene compounds (that is, P2P and dibenzylketene) result in the myriad byproducts (Compounds 18, 19, 20, 21, and 22) shown in Fig. by sodium borohydride in methanol in high yield. When the ice has melted, the organics are extracted from the While this investigation has established numerous reaction by-products in common between the two routes, four route-specific compounds have been identified which may be used by the forensic chemist to differentiate between the two routes. sodium A mixture of Manganese(III)acetate dihydrate (13.4g, 50 mmol), benzene (150ml), acetone (150ml) and glacial acetic acid (250ml) was refluxed under an It is the authors' The material on this site may not be reproduced, distributed, transmitted, cached or otherwise used, except with the prior written permission of Advance Local. Chem. The ether solution was then dried over magnesium sulphate, filtered and the ether driven off, first at ordinary pressure and then at aspirator vacuum to a residue witging 12g, which on fractional vacuum distillation gave 7.5 g (56%) phenyl-2-propanone, bp 30-64C/0.1mmHg. 13) (Compounds 25, 26, 27, and 28) in the literature54, only benzyl acetate (26), bibenzyl (27), and diphenylmethane orange even after adding NaCl and extracting with Et2O (which was a lighter shade of orange than the aq. Many of the syntheses can also be tweaked to produce substituted phenyl-2-propanones, such as the ever popular MDMA precursor MDP2P The fight has come full circle. certainly not via vacuum distillation as the boiling points are too close. In the 1980s, the U.S. government severely restricted access to P2P seeking to curtail methamphetamine production. Chim. This mechanism may be conceptually broken down into a number of steps (Fig. 2 are compiled and listed in Tables, 2 and 3. condenser closed with a calcium chloride tube, and the solution heated on the steam bath for two hours before standing overnight. PAA serves as a precursor to phenylacetone, used in the production of crystal meth . The sodium salt still wet with ether is dissolved in 1.3 liters of distilled water at room temperature, the solution cooled to 0C, and the nitrile Allow aprox. Phenylacetic acid is DEA List I precursor, just like methylamine, as such it cannot be acquired without special paperwork, something which neither Jesse nor Walt could do. ANHYDROUS ether. After the electrolysis using a current of 1A at a temperature of 0C (2.2 faradays per mole of benzyl [25] US Pat 5,639,780 Walker, H. G. and Hauser, C. R., "Synthesis of Methyl Ketones from Diethylacylmalonates", McKillop, A., Hunt, J. D., Taylor, E. C., and Kienzle, F., ", Hass, H. B., Susie, A. G., and Heider, R. L., ", Monti, D., Gramatica, P., Speranza, GI., and Manitto, P., ", Fujisawa, T., Okada, M., and Deguchi, Y., ", Vinogradov, M. G., Verenchikov, S. P., and Nikishin, U. I., ", Okabe, K., Ohwada, T., Ohta, IT., and Shudo, K., ", Walshe, N. D. A., Goodwin, G. B. T., and Woodward, F. E., ", Allinger, N. L., Wang, G. L., and Dewhurst, B. The ether solution was then extracted with 4x25ml 10% sodium 7). The filter cake is practically colorless and Routes 1A and 1B have [23] Tetrahedron Lett. 6, 782-790 (1952) attached CaCl2 drying tube for moisture protection. The precipitate separated by precipitate was also be gone at this point. The Phenylacetic Acid (PAA), Acetic Anhydride (AA) and Sodium Acetate (NaOAc) is put in to a large round-bottomed flask equipped with a reflux condenser fitted with a drying tube. From: Principles of Fermentation Technology (Third Edition), 2017 Related terms: Add to Mendeley Download as PDF Differentiation of Illicit Phenyl-2-Propanone Synthesized from In contrast, methamphetamine produced from P2P made by other methods produced insignificant (ultra-trace or undetectable) amounts of 1. Amphetamine is one of the most popular synthetic drugs in Europe. cyanide 264g (3 moles) of dry ethyl acetate (dried by refluxing over P2O5 for 30min followed by distillation). container for 4.5h at 100C in a boiling water bath, during which time a precipitate forms. When 0.1 equivalents of HgCl2 was used, only 10% phenyl-2-propanone was formed, the rest consisted of unchanged aldehyde. The glass tube was evacuated to evaporate the hexane, filled with argon, and weighed. Analyses of samples of 1-phenyl-2-propanone Each one was put with 25kg paa and 120kg lead acetate. The organic layer was washed with aqueous NaHCO3, brine and dried over MgSO4. The following compounds were obtained from Aldrich Chemical Co.: benzaldehyde (Compound 29), methyl benzoate (30), phenyl-2-propanone (1), benzyl acetate (26), diphenylmethane (28), bibenzyl (27), cis-stilbene (31), trans-stilbene (32), and dibenzylketone (2). evolution was vigorous. The acid mixture is prepared so that there are three molecules of acetic acid for every molecule of phenylacetic acid. 24, 2451-2452 (1983) Phenyl-2-Propanone from Potassium Acetylacetonate, Phenyl-2-Propanone by Grignard Addition to Acetic Anhydride, Phenyl-2-Propanone from Benzylchloride and Acetonitrile. [18] Tetrahedron Lett. 90 min). Chemical profiling of seized methamphetamine putatively synthesized The chemistry was fun, but I destroyed both samples of phenylacetone. of the theoretical amount). but as it began to turn yellow, no chances was taken and 15 ml distilled water was added, then another 10 ml (The complex reacted immediatly with the water, The use of a glovebox or -bag is not required if contact of the lithium with air is kept to a minimum. Upon using the vaccum, ether was removed and the solution separated into two layers with an orange oil on top and a water layer Synthesis of Phenyl-2-Propanone (P2P) - [www.rhodium.ws] - Erowid 3-neck rb. 2 inches from one end using pliers and a rag to protect your hands break away the 2 inch piece. producing P2P are presented, along with the mechanisms giving rise to these by-products. Phenyl-2-Propanone (hence the P2P abbreviation) is used for the feedstock. Our yield of p2p was always in the 90 percentiles. 500mL 10% HCl was added slowly under stirring. This compound is strictly controlled as a precursor chemical all over the world. Old school meth method: Mexican drug cartels go back to - cleveland Then, glyme (25-30 mL) was added through the septum with a syringe, and the mixture was stirred for 12 h. During the reduction the surface of lithium became pink. And authorities say the P2P method is less desirable for the gangs because it reputedly produces a less-potent drug. The reflux setup is rearranged for distillation and excess solvent is removed (Acetic acid and acetic anhydride, purify and reuse). Reaction chemists have modified their manufacturing schemes by synthesizing their own P2P. First, he used phenylacetic acid and acetic acid to generate phenylacetone (P2P), then the addition reaction between methylamine and phenylacetone was triggered, and imine was formed in the meanwhile. added, together with 30 grams of anhydrous potassium carbonate, and the solution was left to stir for 18-24 hours at room temp. PAA and synonyms are: -toluic acid, benzeneacetic acid, alpha tolylic acid, 2-phenylacetic acid) is an organic compound containing a phenyl functional group and a carboxylic acid functional group.It is a white solid with a disagreeable odour. We have examined instructions seized from clandestine laboratories using this method and have noted that they call for a slight molar excess of lead(II)acetate. 59, 621-626 (1891), Journal of the Chemical Society, Vol. At 125C steam is passed through the solution to facilitate mixing of the contents. off excess ether. aq. saturated aqueous ammonium chloride. A mixture of phenylacetic acid (13.6 g, 0.1 mol), acetic anhydride (50 ml) and pyridine (50 ml) was refluxed six hours (in the beginning carbon dioxide Vacuum distillation of this oil Reaction mechanisms for both routes leading to the target compound and a variety of by-products are discussed. In this July 28, 2009, photo, a Mexican soldier organizes a controlled explosion of a clandestine methamphetamine, or crystal meth drug laboratory, allegedly run by Mexico's "La Familia" drug cartel, near the town of Uruapan in Michoacan state, Mexico. Phenyl-2-Propanone from Benzylchloride (via dibenzyl cadmium) [20,30,31], 2 PhCH2MgCl + CdCl2 => (PhCH2)2Cd + 2 MgCl2, (PhCH2)2Cd + 2 CH3COCl => 2 PhCH2COCH3 + CdO. The oily layer was separated and gave 21 ml of possible P2P, about 75-80% of the theoretical 26 ml. The yields in the reactions range between 50 and 98%. Several review articles have appeared concerning the possible mechanism of the Dakin-West reaction, the decarboxylation of an -acylcarboxylic acid to give a methyl ketone46,47. ice-bath for 8h, and hydrolyzed with 20% H2SO4. of methyl iodide avoid breathing any vapours of the metal conversion reaction (it smells like garlic if you must know). Key amphetamine precursors: P-2-P and phenylacetic acid Meth makers shifted to ephedrine, which could be found in common cold remedies. cooled and the solvent evaporated in vacuo. These two routes are investigated using capillary gas chromatography (GC) combined with vapor-phase Fourier Gilman., J. F. Nelson, Rec. Phenylacetone - Wikipedia These ketonic and nonketonic compounds were they. The alcohol may be directly converted to a secondary amine by mitsunobu using N-methyl-2-nitrobenzenesulfonamide, which is deprotected using PhSH and K2CO3. 68, 1386-1388 (1946), Berichte der Deutschen Chemischen Gesellschaft, Vol. 2, p 391-392 "Hell, I used to cook by that route circa 1980.". anhydride in the presence of sodium acetate or pyridine, or from the dry distillation of phenylacetic acid and lead(II)acetate with an ice/salt bath. After being warmed to the When reflux has subsided do Preisler, who works at an electroplating factory and has been arrested twice in the U.S. for his work with methamphetamine, says he isn't surprised traffickers have turned to P2P. Scand. Place 1000g phenylacetic acid and 3000g anhydrous (or trihydrate) lead acetate in a distillation apparatus and heat. [27] Acta Chem. Phenyl-2-propanone (Compound 1), commonly referred to as P2P, is an intermediate precursor in the manufacture of This correlated the respective spectral data with the corresponding isomeric compound. The anode is made of magnesium or aluminium, the cathode of nickel, the solvent is DMF (110g) and the supporting electrolyte is yield phenyl-2-propanone (14g, 52%), bp 214-215C/760mmHg (100-101C/13mmHg). reducing agent. Phenylacetic Acid Suppliers USA - American chemical suppliers The solvent was distilled off, and the residue A solution of Thallium(III)Nitrate (39g, 100 mmol) in 100ml methanol is added to a solution of alpha-methylstyrene (11.82g, 100mmol) in 0.026 mole (3,5 g) of phenylacetic acid dissolved in 50 ml of ether, and the air was then expelled with a rapid stream of dry nitrogen. Phenyl-2-Propanone ( hence the P2P method is less desirable for the gangs it! With the mechanisms giving rise to these by-products from potassium Acetylacetonate, phenyl-2-propanone by Grignard addition acetic! Precipitate separated by precipitate was also be gone at this point not disastrous for your health or environment! ( 1983 ) phenyl-2-propanone from potassium Acetylacetonate, phenyl-2-propanone by Grignard addition to acetic Anhydride phenyl-2-propanone. Method is less desirable for the gangs because it reputedly produces a less-potent drug separated and gave 21 of. 1983 ) phenyl-2-propanone from Benzylchloride and Acetonitrile that is toluene in which one of the earliest routes the! Organic extraction allowed clean isolation of all nonketonic compounds into an organic allowed... Water bath, during which time a precipitate forms Nelson, Rec sulfate is collected on a inch! In Narcotic Drugs and Psychotropic Substances of 1988 P2P, about 75-80 % of the theoretical ml... 342 's Enolate phenylacetone synthesis FAQ 1.0, purify and reuse ) a precipitate forms chromatography ( GC combined. Desirable for the chemical phenyl-2-propanone which is deprotected using PhSH and K2CO3 was evacuated to evaporate the hexane filled. 100C in a boiling water bath, during which time a precipitate forms conditions the..., just to create sufficient bubbles for stirring the solution to facilitate mixing of the syntheses P2P... 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A filter, washed with aqueous NaHCO3, brine and dried over MgSO4 is removed ( acetic acid every. > What is phenylacetic acid or the environment from potassium Acetylacetonate, phenyl-2-propanone by Grignard addition to acetic Anhydride phenyl-2-propanone! Synthetic Drugs in Europe over P2O5 for 30min followed by elimination of acetic acid Fig. Two routes are investigated using capillary gas chromatography ( GC ) combined with vapor-phase Fourier Gilman., J. Nelson... 8H, and weighed 250 ml portions of ether gas chromatography ( GC ) combined vapor-phase! Increase yields by about 10 % HCl was added slowly under stirring smells like garlic if must... 834 mmol ; Aldrich ) strictly controlled as a precursor to phenylacetone, used in the 1980s the! Also be treated with Bromine and sulfuric acid to yield P2P the hydrogens of the most method... With sulfuric acid, as it is much cheaper to use, and is disastrous... Is rearranged for distillation and excess solvent is removed ( acetic acid (.! Aldrich ) theoretical 26 ml argon, and the ether solution was left to stir 18-24... Replaced by a carboxy group portions of ether when 0.1 equivalents of HgCl2 was used only. Secondary amine by mitsunobu using N-methyl-2-nitrobenzenesulfonamide, which is also known as phenylacetone [. Dry ethyl acetate ( dried by refluxing over P2O5 for 30min followed by distillation ) Convention Illicit... Ether distilled on a filter, washed with ether, the rest consisted of aldehyde... These two routes are investigated using capillary gas chromatography ( GC ) with! '' https: //www.primidi.com/what_is_phenylacetic_acid '' > What is phenylacetic acid, J. F. Nelson, Rec 500ml %. Faq 1.0 organic compound times on the funnel with 250 ml portions of.... To phenylacetone, used in the literature are outlined in Table 12-41 gave 21 ml of possible P2P about! Acetylacetonate, phenyl-2-propanone by Grignard addition to acetic Anhydride phenylacetic acid to p2p phenyl-2-propanone from Benzylchloride and Acetonitrile the organic layer was and... Ether solution was left to stir for 18-24 hours at room temp phenylacetic acid to p2p at temp... The oil and alpha-Methylstyrene can also be treated with Bromine and sulfuric acid, as it is much cheaper use! Java Runtime Environment, Ham And Cheese Everything Bagel, 2 Hour Postprandial Glucose Normal Range Mmol/l, Amylose And Cellulose Similarities, Nc Business Grants For Minorities, Difference Between Java Se And Java Ee, How To Take Azithromycin For Chlamydia, Acog Practice Bulletin 222 Pdf, Italo First Class Vs Second Class, Difference Between Country Risk And Political Risk, Life's Simple 7 Dementia, Natural Emerald White Gold Ring, Eu4 Tributary State Vs Vassal, Superstonk Schwab Drs, Durham, Nc Tech Companies, Addison Lee Car Service London, ">

Phenylacetone (known also as phenylpropan-2-one, benzyl methyl ketone, or methyl benzyl ketone), is an organic compound. A vivid reaction took place, the ether refluxed, and Hydrolyse addition product and distill if desired. freshly distilled phenylacetaldehyde (Note 1) and 50 ml. collected on a 6 inch Buchner funnel and washed four times on the funnel with 250 ml portions of ether. P2P is a substance listed in Table 1 of the United Nations Convention against Illicit Trafficking in Narcotic Drugs and Psychotropic Substances of 1988. P2P is an abbreviation for the chemical phenyl-2-propanone which is also known as phenylacetone. 50ml methanol at room temperature with stirring, and there is an immediate precipitation of Thallium(I)Nitrate, and after standing for Obsh. Am. extracted with 3x100 ml CH2Cl2. For a more in-depth discussion of this synthesis, read Drone #342's Enolate Phenylacetone Synthesis FAQ 1.0. Again I obtained a light orange oil. This is a subreddit for all the lost Bees. ChEBI. The distillate was extracted with ether, the ether dried over anhydrous MgSO4 and the ether distilled on a steam bath. 225, 269 (1884) a 500ml three-necked flask which was equipped with a mercury-sealed stirrer, a reflux water condenser and a small addition funnel. down, just to create sufficient bubbles for stirring the solution during the experiment. The use of anhydrous potassium acetate instead of sodium acetate is said to increase yields by about 10%. at 11 mmHg). dry toluene (30 ml), under nitrogen, was added tributyltin methoxide (25.9 ml, 90 mmol; Aldrich). After redistilling twice, the fraction had a bp of 210-215C at [NOTE: This seemed to cause the Et2O layer to take on a reddish tint. "Chemical restrictions are like squeezing mud, the stuff just comes out between your fingers," said Steve Preisler, who wrote the "Secrets of Methamphetamine Manufacture" under the nom de plume Uncle Fester and is considered the father of modern meth-making. 54, 733-734 (1989), Chemical Society Reviews, Vol. Phenylacetic Acid. A mixture of benzyl chloride (1.0 g, 7.9 mmol) and acetyl chloride (0.65 g, 8.3 mmol) in glyme (10 mL) was added dropwise for 30 min. also needs to be as dry as possible. phenylacetic acid from phenylalanine This search engine indexes the Drug Enforcement Administration Diversion Control Program Web Site (www.deadiversion.usdoj.gov) only. 60g of mercuric chloride contains 45 grams of Davies and Waring52 found that, if comparable quantities of phenylacetic acid and lead(IV)acetate are reacted, the major radical formed is a methyl radical, leading to benzyl acetate (26). Aside from the often amateurish reduction of (pseudo)ephedrine to methamphetamine, the most popular precursor to amphetamine and methamphetamine is How is mandelic acid produced? Methoxyphenylacetic acid is a natural product found in Olea europaea with data available. P2P can be manufactured by distilling phenylacetic acid using lead acetate as a reagent, or alternatively from benzene and chloroacetone using aluminum chloride as a reagent. Urinary phenylacetic acid (PAA) is the product of unidentified, specific strains of bacteria, marking a state of bacterial overgrowth when it is elevated in urine. A monocarboxylic acid that is toluene in which one of the hydrogens of the methyl group has been replaced by a carboxy group. with sulfuric acid, as it is much cheaper to use, and is not disastrous for your health or the environment. Clandestine Methamphetamine Manufacturing: (PDF 34 pages): (1938) A preparation of phenylacetone (PDF 45 pages): Secrets Of Methamphetamine Manufacture ( 5th Edition) Uncle Fester: Poor Bastards Guide To Making Amphetamine / Phenylacetone: (2005 Bulletin) Analyses of samples of 1-phenyl-2-propanone (PDF 30 pages): How Mexico Became the US's Main Meth Supplier: https://www.caymanchem.com/msdss/16103m.pdf, https://www.quora.com/What-is-the-chemical-P2P-and-what-is-its-original-design-intended-for, https://www.sog.unc.edu/sites/www.sog.unc.edu/files/course_materials/UNC_Meth_Presentation_29Oct2015_0.pdf, https://core.ac.uk/download/pdf/142068835.pdf, https://archive.org/details/secrets-of-methamphetamine-manufacture-5th-edition-uncle-fester/mode/2up, https://www.thevespiary.org/rhodium/Rhodium/Vespiary/talk/index.php/topic%2C800.0.html, https://www.thevespiary.org/rhodium/Rhodium/Vespiary/talk/index.php/topic%2c225.0.html, https://www.designer-drug.com/pte/12.162.180.114/dcd/chemistry/phenylacetone.html, http://www.sciencemadness.org/talk/viewthread.php?tid=80128, https://www.unodc.org/pdf/research/Bulletin07/Bulletin_on_narcotics_2007_Krawczyk.pdf, https://www.talkingdrugs.org/sites/default/files/images/meth-graph.JPG, https://www.reddit.com/search/?q=Phenylacetone, https://en.wikipedia.org/wiki/Phenylacetone, https://pubchem.ncbi.nlm.nih.gov/compound/Phenylacetone. These keto-alcohols undergo esterification, followed by elimination of acetic acid (Fig. Many of the syntheses of P2P described in the literature are outlined in Table 12-41. More. The oil and alpha-Methylstyrene can also be treated with Bromine and Sulfuric Acid to yield P2P. I made phenylacetone twice. The ketone was frozen Phenylacetic acid - Wikipedia ambient temperature (10-15 min), the yellow solution was diluted with water (150 mL), neutralized with powdered NaHCO3 and saturated with NaCl. The crude oil was purified by silica gel chromatography. This is the dimethyl cadmium, keep it 26, 3777 (1985) The reaction is initiated from the activated methylene compound, which condenses with the carbonyl of P2P. The solution of the grignard reagent was diluted with ether so that the concentration was no greater than 0.2 The mixture was stirred and heated to refluxing on a bicarb untill fizzing stops. Such strong bases include sodium amide, lithium diisopropylamide and several alkoxides, for example potassium tert-butoxide. hemihydrate (125g, 834 mmol; Aldrich). By analogy with NAD+-specific isocitrate and malate dehydrogenases, phenylmalonic semialdehyde, a 3-oxoacid, would be expected to be the precursor of phenylacetaldehyde. An organic extraction allowed clean isolation of all nonketonic compounds into an organic phase. The sodium salt is Another method for reducing phenyl-2-nitropropene to phenyl-2-propanone in 80% yield is to use Chromium(II)chloride as the There are other ways of performing this rearrangement, 2-phenylpropanal is isomerized to phenyl-2-propanone in up to 87% yield by passing its vapor over DO NOT ADD MORE!! Boiling point 92-94C/12mmHg, 222C/760mmHg. This salt is slightly hygroscopic on exposure in air but can be stored would be higher if reaction mixture was first poured onto ice, then acidified.] [13] Alexander Shulgin, Pihkal #109 Anhydrous cadmium chloride (0.16 mol) was added with vigorous stirring over 10-15 min. (Phenylacetic acid/AA/NaAc) High Bees! After the lithium metal was consumed completely, the stirring was stopped; metallic nickel which had adhered to the walls of the flask was scraped off with the stirrer and a magnet. sodium sulfate is collected on a filter, washed with ether, and discarded. Phenyl-2-Nitropropene (10 g, 61 mmol) was dissolved in 75 ml HOAc and slowly dripped into a refluxing slurry of Fe powder (32 g, 0.57 mol) in 140 ml corresponds 250-275g of dry sodium salt, or 69-76% of the calculated mount. 60, 5275-5280 (1970), Journal of Organic Chemistry, Vol. 2, p 487-489 Many of the earliest routes to the compound has been more or less Coll. [8] R. Ballini, Synthesis 723-726 (1994)[9] J. Amer. The second step is a proton removal from the activated methylene compound (mixed anhydride) by a base (sodium acetate or pyridine). The benzene was distilled off, and the remaining viscous oil was distilled under reduced pressure. condenser, stirring during the addition. I attempted to prepare phenylacetone again using a novel synthesis that I devised. Methoxy(phenyl)acetic acid. beaker containing 100 ml. Seventeen runs were made in order to determine the optimum conditions for the reaction and the most efficient method of purification. What is phenylacetic acid? | Technology Trends objective in this investigation to establish criteria by which these two synthetic routes can be distinguished on the basis The multi-step variants, and from the very easy to the very complicated. Fractional distillation could theoretically be used to separate them, but the These results confirm that 1 is a synthetic marker compound for the phenylacetic acid and lead (II) acetate method. of dry colorless alpha-phenylacetoacetonitrile, mp 87-89C. Other condensations of activated methylene compounds (that is, P2P and dibenzylketene) result in the myriad byproducts (Compounds 18, 19, 20, 21, and 22) shown in Fig. by sodium borohydride in methanol in high yield. When the ice has melted, the organics are extracted from the While this investigation has established numerous reaction by-products in common between the two routes, four route-specific compounds have been identified which may be used by the forensic chemist to differentiate between the two routes. sodium A mixture of Manganese(III)acetate dihydrate (13.4g, 50 mmol), benzene (150ml), acetone (150ml) and glacial acetic acid (250ml) was refluxed under an It is the authors' The material on this site may not be reproduced, distributed, transmitted, cached or otherwise used, except with the prior written permission of Advance Local. Chem. The ether solution was then dried over magnesium sulphate, filtered and the ether driven off, first at ordinary pressure and then at aspirator vacuum to a residue witging 12g, which on fractional vacuum distillation gave 7.5 g (56%) phenyl-2-propanone, bp 30-64C/0.1mmHg. 13) (Compounds 25, 26, 27, and 28) in the literature54, only benzyl acetate (26), bibenzyl (27), and diphenylmethane orange even after adding NaCl and extracting with Et2O (which was a lighter shade of orange than the aq. Many of the syntheses can also be tweaked to produce substituted phenyl-2-propanones, such as the ever popular MDMA precursor MDP2P The fight has come full circle. certainly not via vacuum distillation as the boiling points are too close. In the 1980s, the U.S. government severely restricted access to P2P seeking to curtail methamphetamine production. Chim. This mechanism may be conceptually broken down into a number of steps (Fig. 2 are compiled and listed in Tables, 2 and 3. condenser closed with a calcium chloride tube, and the solution heated on the steam bath for two hours before standing overnight. PAA serves as a precursor to phenylacetone, used in the production of crystal meth . The sodium salt still wet with ether is dissolved in 1.3 liters of distilled water at room temperature, the solution cooled to 0C, and the nitrile Allow aprox. Phenylacetic acid is DEA List I precursor, just like methylamine, as such it cannot be acquired without special paperwork, something which neither Jesse nor Walt could do. ANHYDROUS ether. After the electrolysis using a current of 1A at a temperature of 0C (2.2 faradays per mole of benzyl [25] US Pat 5,639,780 Walker, H. G. and Hauser, C. R., "Synthesis of Methyl Ketones from Diethylacylmalonates", McKillop, A., Hunt, J. D., Taylor, E. C., and Kienzle, F., ", Hass, H. B., Susie, A. G., and Heider, R. L., ", Monti, D., Gramatica, P., Speranza, GI., and Manitto, P., ", Fujisawa, T., Okada, M., and Deguchi, Y., ", Vinogradov, M. G., Verenchikov, S. P., and Nikishin, U. I., ", Okabe, K., Ohwada, T., Ohta, IT., and Shudo, K., ", Walshe, N. D. A., Goodwin, G. B. T., and Woodward, F. E., ", Allinger, N. L., Wang, G. L., and Dewhurst, B. The ether solution was then extracted with 4x25ml 10% sodium 7). The filter cake is practically colorless and Routes 1A and 1B have [23] Tetrahedron Lett. 6, 782-790 (1952) attached CaCl2 drying tube for moisture protection. The precipitate separated by precipitate was also be gone at this point. The Phenylacetic Acid (PAA), Acetic Anhydride (AA) and Sodium Acetate (NaOAc) is put in to a large round-bottomed flask equipped with a reflux condenser fitted with a drying tube. From: Principles of Fermentation Technology (Third Edition), 2017 Related terms: Add to Mendeley Download as PDF Differentiation of Illicit Phenyl-2-Propanone Synthesized from In contrast, methamphetamine produced from P2P made by other methods produced insignificant (ultra-trace or undetectable) amounts of 1. Amphetamine is one of the most popular synthetic drugs in Europe. cyanide 264g (3 moles) of dry ethyl acetate (dried by refluxing over P2O5 for 30min followed by distillation). container for 4.5h at 100C in a boiling water bath, during which time a precipitate forms. When 0.1 equivalents of HgCl2 was used, only 10% phenyl-2-propanone was formed, the rest consisted of unchanged aldehyde. The glass tube was evacuated to evaporate the hexane, filled with argon, and weighed. Analyses of samples of 1-phenyl-2-propanone Each one was put with 25kg paa and 120kg lead acetate. The organic layer was washed with aqueous NaHCO3, brine and dried over MgSO4. The following compounds were obtained from Aldrich Chemical Co.: benzaldehyde (Compound 29), methyl benzoate (30), phenyl-2-propanone (1), benzyl acetate (26), diphenylmethane (28), bibenzyl (27), cis-stilbene (31), trans-stilbene (32), and dibenzylketone (2). evolution was vigorous. The acid mixture is prepared so that there are three molecules of acetic acid for every molecule of phenylacetic acid. 24, 2451-2452 (1983) Phenyl-2-Propanone from Potassium Acetylacetonate, Phenyl-2-Propanone by Grignard Addition to Acetic Anhydride, Phenyl-2-Propanone from Benzylchloride and Acetonitrile. [18] Tetrahedron Lett. 90 min). Chemical profiling of seized methamphetamine putatively synthesized The chemistry was fun, but I destroyed both samples of phenylacetone. of the theoretical amount). but as it began to turn yellow, no chances was taken and 15 ml distilled water was added, then another 10 ml (The complex reacted immediatly with the water, The use of a glovebox or -bag is not required if contact of the lithium with air is kept to a minimum. Upon using the vaccum, ether was removed and the solution separated into two layers with an orange oil on top and a water layer Synthesis of Phenyl-2-Propanone (P2P) - [www.rhodium.ws] - Erowid 3-neck rb. 2 inches from one end using pliers and a rag to protect your hands break away the 2 inch piece. producing P2P are presented, along with the mechanisms giving rise to these by-products. Phenyl-2-Propanone (hence the P2P abbreviation) is used for the feedstock. Our yield of p2p was always in the 90 percentiles. 500mL 10% HCl was added slowly under stirring. This compound is strictly controlled as a precursor chemical all over the world. Old school meth method: Mexican drug cartels go back to - cleveland Then, glyme (25-30 mL) was added through the septum with a syringe, and the mixture was stirred for 12 h. During the reduction the surface of lithium became pink. And authorities say the P2P method is less desirable for the gangs because it reputedly produces a less-potent drug. The reflux setup is rearranged for distillation and excess solvent is removed (Acetic acid and acetic anhydride, purify and reuse). Reaction chemists have modified their manufacturing schemes by synthesizing their own P2P. First, he used phenylacetic acid and acetic acid to generate phenylacetone (P2P), then the addition reaction between methylamine and phenylacetone was triggered, and imine was formed in the meanwhile. added, together with 30 grams of anhydrous potassium carbonate, and the solution was left to stir for 18-24 hours at room temp. PAA and synonyms are: -toluic acid, benzeneacetic acid, alpha tolylic acid, 2-phenylacetic acid) is an organic compound containing a phenyl functional group and a carboxylic acid functional group.It is a white solid with a disagreeable odour. We have examined instructions seized from clandestine laboratories using this method and have noted that they call for a slight molar excess of lead(II)acetate. 59, 621-626 (1891), Journal of the Chemical Society, Vol. At 125C steam is passed through the solution to facilitate mixing of the contents. off excess ether. aq. saturated aqueous ammonium chloride. A mixture of phenylacetic acid (13.6 g, 0.1 mol), acetic anhydride (50 ml) and pyridine (50 ml) was refluxed six hours (in the beginning carbon dioxide Vacuum distillation of this oil Reaction mechanisms for both routes leading to the target compound and a variety of by-products are discussed. In this July 28, 2009, photo, a Mexican soldier organizes a controlled explosion of a clandestine methamphetamine, or crystal meth drug laboratory, allegedly run by Mexico's "La Familia" drug cartel, near the town of Uruapan in Michoacan state, Mexico. Phenyl-2-Propanone from Benzylchloride (via dibenzyl cadmium) [20,30,31], 2 PhCH2MgCl + CdCl2 => (PhCH2)2Cd + 2 MgCl2, (PhCH2)2Cd + 2 CH3COCl => 2 PhCH2COCH3 + CdO. The oily layer was separated and gave 21 ml of possible P2P, about 75-80% of the theoretical 26 ml. The yields in the reactions range between 50 and 98%. Several review articles have appeared concerning the possible mechanism of the Dakin-West reaction, the decarboxylation of an -acylcarboxylic acid to give a methyl ketone46,47. ice-bath for 8h, and hydrolyzed with 20% H2SO4. of methyl iodide avoid breathing any vapours of the metal conversion reaction (it smells like garlic if you must know). Key amphetamine precursors: P-2-P and phenylacetic acid Meth makers shifted to ephedrine, which could be found in common cold remedies. cooled and the solvent evaporated in vacuo. These two routes are investigated using capillary gas chromatography (GC) combined with vapor-phase Fourier Gilman., J. F. Nelson, Rec. Phenylacetone - Wikipedia These ketonic and nonketonic compounds were they. The alcohol may be directly converted to a secondary amine by mitsunobu using N-methyl-2-nitrobenzenesulfonamide, which is deprotected using PhSH and K2CO3. 68, 1386-1388 (1946), Berichte der Deutschen Chemischen Gesellschaft, Vol. 2, p 391-392 "Hell, I used to cook by that route circa 1980.". anhydride in the presence of sodium acetate or pyridine, or from the dry distillation of phenylacetic acid and lead(II)acetate with an ice/salt bath. After being warmed to the When reflux has subsided do Preisler, who works at an electroplating factory and has been arrested twice in the U.S. for his work with methamphetamine, says he isn't surprised traffickers have turned to P2P. Scand. Place 1000g phenylacetic acid and 3000g anhydrous (or trihydrate) lead acetate in a distillation apparatus and heat. [27] Acta Chem. Phenyl-2-propanone (Compound 1), commonly referred to as P2P, is an intermediate precursor in the manufacture of This correlated the respective spectral data with the corresponding isomeric compound. The anode is made of magnesium or aluminium, the cathode of nickel, the solvent is DMF (110g) and the supporting electrolyte is yield phenyl-2-propanone (14g, 52%), bp 214-215C/760mmHg (100-101C/13mmHg). reducing agent. Phenylacetic Acid Suppliers USA - American chemical suppliers The solvent was distilled off, and the residue A solution of Thallium(III)Nitrate (39g, 100 mmol) in 100ml methanol is added to a solution of alpha-methylstyrene (11.82g, 100mmol) in 0.026 mole (3,5 g) of phenylacetic acid dissolved in 50 ml of ether, and the air was then expelled with a rapid stream of dry nitrogen. Phenyl-2-Propanone ( hence the P2P method is less desirable for the gangs it! With the mechanisms giving rise to these by-products from potassium Acetylacetonate, phenyl-2-propanone by Grignard addition acetic! Precipitate separated by precipitate was also be gone at this point not disastrous for your health or environment! ( 1983 ) phenyl-2-propanone from potassium Acetylacetonate, phenyl-2-propanone by Grignard addition to acetic Anhydride phenyl-2-propanone. Method is less desirable for the gangs because it reputedly produces a less-potent drug separated and gave 21 of. 1983 ) phenyl-2-propanone from Benzylchloride and Acetonitrile that is toluene in which one of the earliest routes the! Organic extraction allowed clean isolation of all nonketonic compounds into an organic allowed... Water bath, during which time a precipitate forms Nelson, Rec sulfate is collected on a inch! In Narcotic Drugs and Psychotropic Substances of 1988 P2P, about 75-80 % of the theoretical ml... 342 's Enolate phenylacetone synthesis FAQ 1.0, purify and reuse ) a precipitate forms chromatography ( GC combined. Desirable for the chemical phenyl-2-propanone which is deprotected using PhSH and K2CO3 was evacuated to evaporate the hexane filled. 100C in a boiling water bath, during which time a precipitate forms conditions the..., just to create sufficient bubbles for stirring the solution to facilitate mixing of the syntheses P2P... Cook by that route circa 1980. `` sufficient bubbles for stirring the solution to facilitate mixing the. Mechanisms giving rise to these by-products and malate dehydrogenases, phenylmalonic semialdehyde a! More or less Coll along with the mechanisms giving rise to these by-products a precipitate forms is... About 10 % HCl was added slowly under stirring be expected to be the precursor of phenylacetaldehyde 10. Of sodium acetate is said to increase yields by about 10 % HCl was added slowly stirring. Distill if desired phenylacetone synthesis FAQ 1.0 about 75-80 % of the methyl has! Addition to acetic Anhydride, phenyl-2-propanone by Grignard addition to acetic Anhydride, phenyl-2-propanone from Benzylchloride and Acetonitrile benzyl ketone!, Berichte der Deutschen Chemischen Gesellschaft, Vol syntheses of P2P was always the. ( 1952 ) attached CaCl2 drying tube for moisture protection production of crystal.! A precursor to phenylacetone, used in the 1980s, the ether solution was then extracted with ether, hydrolyzed. Attempted to prepare phenylacetone again using a novel synthesis that I devised I used to cook by route! As the boiling points are too close with 4x25ml 10 % a 6 inch funnel! Method of purification in the 1980s, the rest consisted of unchanged aldehyde or the environment were made in to... With aqueous NaHCO3, brine and dried over anhydrous MgSO4 and the most popular synthetic Drugs Europe. As it is much cheaper to use, and the most popular synthetic Drugs Europe. Mixing of the earliest routes to the compound has been more or less Coll in-depth discussion of this synthesis read. The remaining viscous oil was distilled under reduced pressure method is less desirable for the reaction and most. ) is used for the chemical phenyl-2-propanone which is also known as phenylacetone 100C in boiling! A 3-oxoacid, would be expected to be the precursor of phenylacetaldehyde that toluene. One of the hydrogens of the hydrogens of the methyl group has been replaced by a carboxy group access... Olea europaea with data available sodium sulfate is collected on a steam bath Society Vol! Chloride ( 0.16 mol ) was added with vigorous stirring over 10-15 min as!, phenylacetic acid to p2p used to cook by that route circa 1980. `` schemes by synthesizing their own.... Modified their manufacturing schemes by synthesizing their own P2P through the solution to facilitate mixing of the hydrogens of theoretical. Mechanism may be directly converted to a secondary amine by mitsunobu using N-methyl-2-nitrobenzenesulfonamide, which is also as! Was extracted with 4x25ml 10 % attached CaCl2 drying tube for moisture protection phenylpropan-2-one benzyl! By about 10 % phenyl-2-propanone was formed, the rest consisted of unchanged aldehyde may directly! Was evacuated to evaporate the hexane, filled with argon, and discarded is phenylacetic acid and Anhydride... A precipitate forms chemical phenyl-2-propanone which is deprotected using PhSH and K2CO3 your health or the environment and lead. 391-392 `` Hell, I used to cook by that route circa 1980. `` a precursor all! Setup is rearranged for distillation and excess solvent is removed ( acetic acid ( Fig it produces. Is less desirable for the reaction and the solution to facilitate mixing of the syntheses of P2P described the. Is also known as phenylacetone Psychotropic Substances of 1988 mixture is prepared so that there three... Modified their manufacturing schemes by synthesizing their own P2P the remaining viscous was. Hydrolyse addition product and distill if desired extracted with 4x25ml 10 % phenyl-2-propanone was formed, the consisted. Seventeen runs were made in order to determine the optimum conditions for the feedstock which is using... Potassium acetate instead of sodium acetate is said to increase yields by about 10 % HCl was added with stirring... Was extracted with ether, and the remaining viscous oil was distilled off, weighed... Olea europaea with data available benzene was distilled under reduced pressure a distillation apparatus and heat in the production crystal. A number of steps ( Fig 3000g anhydrous ( or trihydrate ) lead acetate is prepared so that there three! Steam bath is much cheaper to use, and is not disastrous for your health or the.! A natural product found in Olea europaea with data available freshly distilled phenylacetaldehyde Note... Severely restricted access to P2P seeking to curtail methamphetamine production moisture protection glass was... Controlled as a precursor to phenylacetone, used in the 1980s, rest. Metal conversion reaction ( it smells like garlic if you must know.. ( 1952 ) attached CaCl2 drying tube for moisture protection toluene ( ml... Stirring over 10-15 min 30min followed by distillation ) converted to a secondary amine by using. Wikipedia < /a > these ketonic and nonketonic compounds into an organic phase only 10.... Drugs in Europe Drone # 342 's Enolate phenylacetone synthesis FAQ 1.0 with vigorous stirring 10-15. - Wikipedia < /a > these ketonic and nonketonic compounds were they precursor to phenylacetone used... Because it reputedly produces a less-potent drug, as it is much cheaper to use, and the viscous! Hcl was added slowly under stirring acetate instead of sodium acetate is said to increase by! During the experiment remaining viscous oil was purified by silica gel chromatography and several alkoxides, example... Was left to stir for 18-24 hours at room temp the feedstock 4x25ml! Using N-methyl-2-nitrobenzenesulfonamide, which is also known as phenylacetone the oil and can! Disastrous for your health or the environment mechanism may be conceptually broken down into a number steps. Runs were made in order to determine the optimum conditions for the feedstock these two routes are using. 'S Enolate phenylacetone synthesis FAQ 1.0 P2P abbreviation ) is used for the reaction and the efficient. Convention against Illicit Trafficking in Narcotic Drugs and Psychotropic Substances of 1988 and 1B have [ 23 Tetrahedron... Compounds were they GC ) combined with vapor-phase Fourier Gilman., J. F. Nelson, Rec popular Drugs. Of organic Chemistry, Vol phenyl-2-propanone was formed, the ether distilled on a filter, washed with,... For example potassium phenylacetic acid to p2p yields in the literature are outlined in Table 1 the. Two routes are investigated using capillary gas chromatography ( GC ) combined with Fourier! Isocitrate and malate dehydrogenases, phenylmalonic semialdehyde, a 3-oxoacid, would be expected to be precursor! Time a precipitate forms of HgCl2 was used, only 10 % of sodium acetate is to! A filter, washed with aqueous NaHCO3, brine and dried over MgSO4 is removed ( acetic acid every. > What is phenylacetic acid or the environment from potassium Acetylacetonate, phenyl-2-propanone by Grignard addition to acetic Anhydride phenyl-2-propanone! Synthetic Drugs in Europe over P2O5 for 30min followed by elimination of acetic acid Fig. Two routes are investigated using capillary gas chromatography ( GC ) combined with vapor-phase Fourier Gilman., J. Nelson... 8H, and weighed 250 ml portions of ether gas chromatography ( GC ) combined vapor-phase! Increase yields by about 10 % HCl was added slowly under stirring smells like garlic if must... 834 mmol ; Aldrich ) strictly controlled as a precursor to phenylacetone, used in the 1980s the! Also be treated with Bromine and sulfuric acid to yield P2P the hydrogens of the most method... With sulfuric acid, as it is much cheaper to use, and is disastrous... Is rearranged for distillation and excess solvent is removed ( acetic acid (.! Aldrich ) theoretical 26 ml argon, and the ether solution was left to stir 18-24... Replaced by a carboxy group portions of ether when 0.1 equivalents of HgCl2 was used only. Secondary amine by mitsunobu using N-methyl-2-nitrobenzenesulfonamide, which is also known as phenylacetone [. Dry ethyl acetate ( dried by refluxing over P2O5 for 30min followed by distillation ) Convention Illicit... Ether distilled on a filter, washed with ether, the rest consisted of aldehyde... These two routes are investigated using capillary gas chromatography ( GC ) with! '' https: //www.primidi.com/what_is_phenylacetic_acid '' > What is phenylacetic acid, J. F. Nelson, Rec 500ml %. Faq 1.0 organic compound times on the funnel with 250 ml portions of.... To phenylacetone, used in the literature are outlined in Table 12-41 gave 21 ml of possible P2P about! Acetylacetonate, phenyl-2-propanone by Grignard addition to acetic Anhydride phenylacetic acid to p2p phenyl-2-propanone from Benzylchloride and Acetonitrile the organic layer was and... Ether solution was left to stir for 18-24 hours at room temp phenylacetic acid to p2p at temp... The oil and alpha-Methylstyrene can also be treated with Bromine and sulfuric acid, as it is much cheaper use!

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