Everyone says this method has flaws. Has anyone ever really gotten significant yields with this method?
- By Ortist
I 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
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- By Ortist
You 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…
- By lalalander
That'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.
- By lalalander
Unless 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
Their 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
Also 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
There 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
1 - 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
1. 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
Thank 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
OK, and I didn't distill anything. Not MPB, acetoxy, or my P2P, but my downside was that I didn't do the saponification of acetoxy, right. No when I did it right, I got 13 g of dark orange P2P, that I washed a'la Uncle Fester. I got so clean P2P that I see through it. Annnd, it worked in my Leuckart with formamide plus ammonium formate catalyst, and ZnCl2-catalyst (it can be used). I have the better, AlCl3-catalyst for Leuckart, but I was thinking that have I made it wrong. So, with right purification (I purified my acetoxy also, and got clean very sweet smelling yellow oil. And, I read that PDF when they didn't distill P2P and tested the impurities, in P2P, there was impurities, but in VERY low amount.
I do not have even distilling apparatus anymore, because those cheap apparatus i bought, breaks very easily. For example, my magnetic stirrer broke, in my heating mantle, the first week, if I remember correctly. So, I have to buy one whole setup again. Now I have just erlenmeyer, broken glass stick, reflux column, and heating mantle. I also broke my 100 ml measuring flask. DAMN!
Can someone give me advise what kind of apparatus I have to buy to make the vacuum for distilling. I have vacuum holes in those glassses. And they are $24/40. What it means, I don't really know, I think that means the vacuum amount, or what?!
I do not have even distilling apparatus anymore, because those cheap apparatus i bought, breaks very easily. For example, my magnetic stirrer broke, in my heating mantle, the first week, if I remember correctly. So, I have to buy one whole setup again. Now I have just erlenmeyer, broken glass stick, reflux column, and heating mantle. I also broke my 100 ml measuring flask. DAMN!
Can someone give me advise what kind of apparatus I have to buy to make the vacuum for distilling. I have vacuum holes in those glassses. And they are $24/40. What it means, I don't really know, I think that means the vacuum amount, or what?!