Everyone says this method has flaws. Has anyone ever really gotten significant yields with this method?
- By Ortist
lalalanderI used this method many times. Modified a bit. The best results I got was 30ml of P2P from 100ml of benzaldehyde. Also I know a few people who researched this reaction alot; their best results were around 35ml of P2P.
Working method:
1. Methyl-phenyl-butenone prepared as follows: 500ml of benzaldehyde is mixed with 1000ml of MEK. Mixture is cooled in a bucked filled with ice to around +5 degrees.
2. To this is added aqueous HCL, 35-37%, (you have to add 100g of pure HCL which corresponds to about 286ml of 37%HCL)
3. Mix and keep it in a bucket with ice overnight, let the ice melt.
4. Wait 24 hours more
5. Put it in a separatory funnel, discard lower layer.
6. Wash the dark brown-red mixture with 500ml of water, discard water.
7. Distill everything that boils below 150 degrees at atmosferic pressure and discard
8. Distill the rest in vacuum to get a yellow oil
This oil will darken on standing within a week.
Bayer-Villiger:
1. 100ml of above prepared oil add to mixture of 300ml of glacial acetic acid and 100ml of 50% hydrogen peroxide.
2. Heat & stir it at 55 degrees.
3. When reaction starts temperature will go up above 55..60 (about 1..2 hours) : this is the indication to turn OFF heating. If temperaturfe climbs to 70 then cool your flask under running water a bit.
4. Stir until temperature falls back to 50..55 degrees, then turn heating ON again
5. Stir & heat for 6 hours
7. Pour mixture to 1L of water, extract 3 times with 100+100+100ml of DCM
8. Distill DCM off
Saponification:
1. Put Bayer-Villiger product from the step above in a flask with stirring. Slowly add
NaOH solution (30g NaOH, 250ml water, 250ml ethanol). Slowly means dropwise, about 3..5 drops a second. Mixture becomes reddish-orange
2. At the end of addition pH should be above 12
3. To the mixture add acetic acid (any percentage) until neutral pH. Mixture will turn yellow
4. Pour this to 1L of water and extract 3 times with 100+100+100ml of DCM
5. Distill DCM & traces of ethanol off at atmospheric pressure
6. Distill your P2P under vacuum.
7. There will be alot of tar left in a flask
Working method:
1. Methyl-phenyl-butenone prepared as follows: 500ml of benzaldehyde is mixed with 1000ml of MEK. Mixture is cooled in a bucked filled with ice to around +5 degrees.
2. To this is added aqueous HCL, 35-37%, (you have to add 100g of pure HCL which corresponds to about 286ml of 37%HCL)
3. Mix and keep it in a bucket with ice overnight, let the ice melt.
4. Wait 24 hours more
5. Put it in a separatory funnel, discard lower layer.
6. Wash the dark brown-red mixture with 500ml of water, discard water.
7. Distill everything that boils below 150 degrees at atmosferic pressure and discard
8. Distill the rest in vacuum to get a yellow oil
This oil will darken on standing within a week.
Bayer-Villiger:
1. 100ml of above prepared oil add to mixture of 300ml of glacial acetic acid and 100ml of 50% hydrogen peroxide.
2. Heat & stir it at 55 degrees.
3. When reaction starts temperature will go up above 55..60 (about 1..2 hours) : this is the indication to turn OFF heating. If temperaturfe climbs to 70 then cool your flask under running water a bit.
4. Stir until temperature falls back to 50..55 degrees, then turn heating ON again
5. Stir & heat for 6 hours
7. Pour mixture to 1L of water, extract 3 times with 100+100+100ml of DCM
8. Distill DCM off
Saponification:
1. Put Bayer-Villiger product from the step above in a flask with stirring. Slowly add
NaOH solution (30g NaOH, 250ml water, 250ml ethanol). Slowly means dropwise, about 3..5 drops a second. Mixture becomes reddish-orange
2. At the end of addition pH should be above 12
3. To the mixture add acetic acid (any percentage) until neutral pH. Mixture will turn yellow
4. Pour this to 1L of water and extract 3 times with 100+100+100ml of DCM
5. Distill DCM & traces of ethanol off at atmospheric pressure
6. Distill your P2P under vacuum.
7. There will be alot of tar left in a flask
↑View previous replies…
- By lalalander
OrtistIt's good to see that there are people who like to help people. Thank you very much.
- By Ortist
lalalanderYou can also distill P2P with water, but it is very slow. However you MUST distill methyl-phenyl-nutenone under vacuum because there is significant amount of crap and MPB will not distill with water
↑View previous replies…
OrtistThat's a shame. Synthesizing nitroethane to get P2NP is starting to look easier. There was someone on the forum who said that he synthesized P2P easily with this benzaldehyde and mek method in high yield.
OrtistI can make phenylacetic acid from benzyl cyanide. I also own ethyl acetate. Does anyone know if potassium ethoxide is used instead of sodium ethoxide in the synthesis of APAAN? My phenylacetic acid has been sitting in the cupboard for half a year already and I don't know which route to try if I want to make phenylacetone. Is the calcium acetate route good? Sorry, I'm tired and feverish again.
- By Ortist
lalalanderstill using it. Others methods require chemicals which I don't have access to. Most promising is APAAN but i don't have sodium cyanide 
- By lalalander
still using it. Others methods require chemicals which I don't have access to. Most promising is APAAN but i don't have sodium cyanide
- By Ortist
lalalanderSyntyhesing nitroethane is a pain in the ass. All methods I know are low yelding messy processes.
- By lalalander
OrtistUnless we see a video about Benzadehit and MEK, it seems that this problem will not be solved. Either the yield rate is unrealistic, or people are making a significant error in synthesizing.
- By Ortist
lalalanderTheir yeld based on crude P2P. They do not distill it. Basically yes you can get 600+ ml ow a brown oil from the reaction published here, but it is only 250..300 ml of real P2P in it. The rest is high boiling tar. This reaction is know since 2006 (google "twodogs aldol") and since that it was researched alot. No much improvements were made.
- By Ortist
lalalanderAlso their method of preparing MPB (first stage) is wrong as well, as reaction takes around 2 days to completion. Otherwise you'll end up with a lot of unreacted benzaldehyde.
Their glacial acetic acid amount is absolutely insane. I understand where it comes from: original twodogs method uses 1:6 MPB:GAA ratio but it is because he was using sodium perborate instead of peroxide and perborate has a poor solubility. If you use GAA/peroxide you can use 1:3..1:4 MPB:GAA mix. Can be even lower but reaction becomes too exotermic.
This method uses 1:10 MPB:GAA which is a waste
Their glacial acetic acid amount is absolutely insane. I understand where it comes from: original twodogs method uses 1:6 MPB:GAA ratio but it is because he was using sodium perborate instead of peroxide and perborate has a poor solubility. If you use GAA/peroxide you can use 1:3..1:4 MPB:GAA mix. Can be even lower but reaction becomes too exotermic.
This method uses 1:10 MPB:GAA which is a waste
- By lalalander
OrtistThere are a few questions that I want to ask and that I can't really find the answer to. Do you mind if I ask?
- By lalalander
Ortist1 - Converting P2P directly to methamphetamine is said to be more high yielding. What do you think about this? Which method should be followed?
2 - What percentage of P2P can we theoretically convert to methamphetamine? Because my general knowledge is about P2NP and I cannot say that I am overly knowledgeable.
3 - And finally, can we describe racemic products as completely worthless to sell?
2 - What percentage of P2P can we theoretically convert to methamphetamine? Because my general knowledge is about P2NP and I cannot say that I am overly knowledgeable.
3 - And finally, can we describe racemic products as completely worthless to sell?
- By Ortist
lalalander1. Borohydride or Al/Hg depending on the amount of P2P. Al/Hg doesn't require dry conditions but it is a messy workup (Al sludge) and loading more than 20..25g of P2P are hard to handle (too exotermic). Can do many Al/Hg flasks in parallel. Borohydride is cleaner procedure but water can hurt yeld alot
2. Around 70% molar. Roughly you will get 1g from 1g
3. I only make racemic and it is a good stuff. More euphoretic, more energy. Racemic could be converted to D-meth but you will loose roughly 50%. L-meth could be turned into racemate again but it is a different story
2. Around 70% molar. Roughly you will get 1g from 1g
3. I only make racemic and it is a good stuff. More euphoretic, more energy. Racemic could be converted to D-meth but you will loose roughly 50%. L-meth could be turned into racemate again but it is a different story
- By lalalander
OrtistThank you. Since it is a bit tedious to get high yields in P2P synthesis, I think I will proceed with the P2NP method by synthesizing nitroethane. I talked to someone who synthesized nitroethane with a high amount of reagent and he said he achieved successful results. I also had a chance to see some pictures. I can't wait to share the result.
- By TheNut22
still using it. Others methods require chemicals which I don't have access to. Most promising is APAAN but i don't have sodium cyanide
- By TheNut22
OrtistThank you Ortist for valuable and clearly good info!
I've been wondering also about that GAA:s absolutely insane amount.
Should I use 80% or 50% H2O2 for the peracetic acid synthesis? Annnnd, is the in-situ reaction good, or should I make the peracetic first with time around a day or two? Many questions, sorry!
I've been wondering also about that GAA:s absolutely insane amount.
Should I use 80% or 50% H2O2 for the peracetic acid synthesis? Annnnd, is the in-situ reaction good, or should I make the peracetic first with time around a day or two? Many questions, sorry!
