P2p from benzaldehyde and mek The ketone is then subjected to a baeyer-villiger type oxidation using a peracid, such as performic, to the corresponding ester then hydrolyzed to form methyl benzyl ketone. A lot of p2p synthesis only get 30 to 50% yield. ). The best results I got was 30ml of P2P from 100ml of benzaldehyde. Modified a bit. Aug 27, 2021 · I used this method many times. Distilled water 2 L is added. 1. Amphetamines (Phenylethylamines) Precursors Feb 28, 2025 · Synthesis Technologies and Analysis. We now report on our investigations into the synthesis of P2P analogues from substituted benzaldehydes via the Baeyer-Villiger route. Org. Then the ester is saponified with a 10% NaOH solution to get p2p in 35% yield based on the amount of MPB, I believe. 5 h at room temperature. 5h at 100°C P2P should be handled in a fume hood to prevent exposure to fumes and vapors. Everything but benzaldehyde is OTC, what i liked most. 10 mmHg is excellent in this case. The lighter color of ther P2P oil the cleaner it is, simple as that, if it'äs still yellow orangish after first vac-distillation then run it once more vac-. Jan 1, 2008 · We have been investigating the impurities formed when phenyl-2-propanone (P2P) 5, a key ATS precursor, is synthesised in three steps; an aldol condensation of benzaldehyde and methyl ethyl ketone Aug 27, 2021 · Benzaldehyde 1000 g and methyl ethyl ketone (MEK) 1000 ml are mixed in 5 L flask, stirred and chilled at 0 °C. HCl gas is bubbled slowly through the mixture for a 1. There is such advantage like a quite high yield conversion (82% from Apr 17, 2008 · This route is a three step synthesis to P2P; an aldol condensation of benzaldehyde and methyl ethyl ketone (MEK), a Baeyer-Villiger reaction and a subsequent ester hydrolysis. We have identified and selectively synthesised several impurities that may be used as route specific markers for this series of synthetic steps. Method A 30g of 2-phenylpropanal is heated together with a mixture of 60g mercuric chloride (HgCl 2 , 1 eq. If it comes in contact with skin, wash the affected area immediately with soap and water. P2P from Benzaldehyde and MEK Here is the conclusion from the research paper the above graphic is taken from: Conclusions. This route is a three step synthesis to P2P; an aldol condensation of benzaldehyde and methyl ethyl ketone (MEK), a Baeyer-Villiger reaction and a subsequent ester hydrolysis. I just managed to stumble onto this reaction in which benzaldehyde is condensed with MEK to form methyl phenyl butanone. Jun 1, 2018 · This route is a three step synthesis to P2P; an aldol condensation of benzaldehyde and methyl ethyl ketone (MEK), a Baeyer-Villiger reaction and a subsequent ester hydrolysis. Avoid mixing P2P with other chemicals or substances, as it may react and produce toxic byproducts. Avoid inhaling or ingesting P2P. Ive also done madelic acid + HI to phenylacetic acid then phenylacetic acid + lead acetate to p2p. bio (Stranger) 08-09-03 06:16 No 452559 : Benzaldehyde + MEK acid catalyzed aldol Hi twodogs and Rhodium. Its ok to do if you do it in bulk like at least 500ml benzaldehyde scale but i wouldn't bother doing it on less a scale than that. Now making benzalacetone is harder that the aldol for the mek route, especially since acetone likes to do the aldol twice, however when using an excess of acetone the reaction gives good yields. Amphetamines (Phenylethylamines) Precursors Jun 5, 2023 · This phenylacetone (P2P) synthesis approach is a simple way how to get phenylacetone from BMK ethyl glycidate and its synthesis from benzaldehyde. 2. 4. As i can just buy MEK and benzaldehyde it is a lot easier to do it that way even though the yield isnt quite as good. ) and 450ml 75% ethanol in a pressure-safe sealed glass container for 4. 75g P2P from 100g of benzaldehyde. Aug 27, 2021 · Benzaldehyde 1000 g and methyl ethyl ketone (MEK) 1000 ml are mixed in 5 L flask, stirred and chilled at 0 °C. PMK ethyl glycidate can be hydrolyzed into P2P. This reaction isn't sensitive to water like BMK methyl glycidate synthesis. The reaction should be carried out in an inert reactor, and the mouth of the reactor should be sealed with an inert stopper (such as LDPE, Teflon, glass, etc. Amphetamines (Phenylethylamines) Precursors Jun 1, 2016 · The synthesis of impurities detected in clandestinely manufactured Amphetamine Type Stimulants (ATS) has emerged as more desirable than simple "fingerprint" profiling. We have been investigating the impurities formed when phenyl-2-propanone (P2P) 5, a key ATS precursor, is synthesised in three steps; an aldol condensation of benzaldehyde and methyl ethyl ketone (MEK); a Baeyer-Villiger Dec 29, 2024 · When 10 grams of Benzaldehyde + 10 grams of MEK and 7 grams of 30. Jun 1, 2023 · That final oil is extremely contaminated so you must vacum distill it properl with att least 22 mm/Hg vacuum source (aspirator will do fine). 5 h. The product distribution is dependent on the amount of MEK used (vida infra) which in the current example was six equivalents. 2 g of benzaldehyde and 3. In this case the aldol reaction is acid catalysed via Jun 1, 2018 · This route is a three step synthesis to P2P; an aldol condensation of benzaldehyde and methyl ethyl ketone (MEK), a Baeyer-Villiger reaction and a subsequent ester hydrolysis. Also I know a few people who researched this reaction alot; their best results were around 35ml of P2P. We have been investigating the impurities formed when phenyl-2-propanone (P2P) 5, a key ATS precursor, is synthesised in three steps; an aldol condensation of benzaldehyde and methyl ethyl ketone (MEK); a Baeyer-Villiger reaction; and ester hydrolysis. 5% aqueous HCl are mixed for 24 hours at room temperature, I obtain an organic layer. The solution is stirred for addition 1. 5 g of acetone are heated with 20 ml of 10% sodium hydroxide solution on a water bath for 1 hour. Feb 28, 2025 · Synthesis Technologies and Analysis. We have investigated the impurities formed in the so-called Baeyer–Villiger pathway which describes the synthesis of P2P in a 60% yield from benzaldehyde in three steps; an aldol condensation of benzaldehyde and MEK; a Baeyer–Villiger reaction and subsequent ester So reduce reading a bit, it is an acid catalyzed aldol condensation of benzaldehyde and MEK, giving methyl phenyl butenone (MPB) Then there is a Baeyer Villiger oxidation of MPB with peroxy acids to the enol ester of p2p. (1970) vol 35, p 3080) Hydrolize et voilà Jun 1, 2016 · The first step in the Baeyer–Villiger pathway is an aldol condensation between benzaldehyde and MEK to form 3-methyl-4-phenyl-3-buten-2-one 3 as shown in Fig. A few are higher yielding. dustillation and you will have a very light yellow colored P2P (which basically means it has The P2P stays in the organic layer, which is then dried over MgSO 4, the solvent removed under vacuum and the residue vacuum distilled to give pure P2P. Methyl-phenyl-butenone prepared as follows: 500ml of benzaldehyde is mixed with 1000ml of MEK. Yeah using different oxidizers can increase it slighly. In the beginning, he thought about an aldol condensation with benzaldehyde and n-propanal, to give a-methylcinnamaldehyde, which could be hydrated to a-methylhydrocinnamaldehyde, a perfect precursor for beckmann rearrangement and Jun 1, 2018 · This route is a three step synthesis to P2P; an aldol condensation of benzaldehyde and methyl ethyl ketone (MEK), a Baeyer-Villiger reaction and a subsequent ester hydrolysis. : Billups, Kramer, Lastomirsky: J. Toluene can be oxidized to benzaldehyde with persulphate: Post 208719 (Osmium: "Re: The easiest synth of benzaldehyde from toluene", Chemistry Discourse) Condense the prepared benzaldehyde with MEK and do the Baeyer-Villiger with K 2 S 2 O 8 - H 2 SO 4 (ref. Chem. Aug 3, 2003 · P2P distillation Yes, P2P can be distilled without vacuum, but you might get 10% better yield by using vacuum. 3. Working method: 1. formedwhenphenyl-2-propanone (P2P)5,akeyATSprecursor,issynthesisedinthree steps; an aldol condensation of benzaldehyde and methyl ethyl ketone (MEK); a Baeyer–Villiger reaction; and ester hydrolysis. Synthesis Technologies and Analysis. We now report on our Feb 4, 2010 · On the search for a new synthesis route to amphetamines, swin was targeting alpha-methylhydrocinnamic amide as intermediate, from where it is just one more step. Feb 28, 2025 · If this would work like in the paper, you can expect ca. Jun 1, 2016 · This route is a three step synthesis to P2P; an aldol condensation of benzaldehyde and methyl ethyl ketone (MEK), a Baeyer-Villiger reaction and a subsequent ester hydrolysis. MEK is dirt cheap, and i think you can distill the 6-10x molar excess that you use after the reaction out and reuse in the next batch aswell. . vjl hhzbjar dcvps tfvdweh pzxlpr jkpje ddoxvn rbjsw ugmkmb yfp huwngl umask geznv jalrhi ktjjhfdt