P2P synthesis from BMK glycidate ethers

[Saul]

this is the preparation of P2P Phenylacetone CAS 103-79-7 made use of BMK Glycidic Acid ( sodium salt ) CAS 5449-12-7 with main ingredient sulfonic acid strength is 75% CAS 7664-38-2
-------------------------------------------------- ------------------------------
we are going to prepare 1 kg of BMK
take a 5 liter double neck flask
add 500ml boiling water . start with the mixer.
now slowly add 1kg of BMK salt. then add 1 liter of sulfonic acid. now connect the reflux and heat the contents of the flask to max temperature. plus minus 130°c. use a powerful mixer
Let it boil in reflux for 4 hours.
take the top layer and pour it into a measuring cup.
let the bottom layer cool and save for next time. ( we have no chemical waste for this preparation method )

now boil 1 liter of water and add it to the measuring cup. use a hand mixer to mix everything.
After mixing for a few minutes, let the measuring cup cool to room temperature.
remove the top white layer (this is water and waste that we don't need)
the bottom layer is P2P purified and ready to use.

ps: in this preparation we don't have to worry about water remaining in our P2P because water weighs less than P2P

ps2: if you keep these ratios, the P2P will have a ph value of 4 .
if you use more sulfonic acid the ph value will drop to 1. Therefore it is not necessary to use too much sulfonic acid.

 

[w2x3f5]

this is the preparation of P2P Phenylacetone CAS 103-79-7 made use of BMK Glycidic Acid ( sodium salt ) CAS 5449-12-7 with main ingredient sulfonic acid strength is 75% CAS 7664-38-2
-------------------------------------------------- ------------------------------
we are going to prepare 1 kg of BMK
take a 5 liter double neck flask
add 500ml boiling water . start with the mixer.
now slowly add 1kg of BMK salt. then add 1 liter of sulfonic acid. now connect the reflux and heat the contents of the flask to max temperature. plus minus 130°c. use a powerful mixer
Let it boil in reflux for 4 hours.
take the top layer and pour it into a measuring cup.
let the bottom layer cool and save for next time. ( we have no chemical waste for this preparation method )

now boil 1 liter of water and add it to the measuring cup. use a hand mixer to mix everything.
After mixing for a few minutes, let the measuring cup cool to room temperature.
remove the top white layer (this is water and waste that we don't need)
the bottom layer is P2P purified and ready to use.

ps: in this preparation we don't have to worry about water remaining in our P2P because water weighs less than P2P

ps2: if you keep these ratios, the P2P will have a ph value of 4 .
if you use more sulfonic acid the ph value will drop to 1. Therefore it is not necessary to use too much sulfonic acid.

T0RI tried your version of the synthesis, but did not use water, the synthesis takes place in microwave irradiation. At a certain moment, the temperature dropped sharply from 110 degrees to 50 degrees, the reaction was still violent. Have you noticed a drop in temperature as carbon dioxide emission starts?

 

[cernalit0000]

I tried your version of the synthesis, but did not use water, the synthesis takes place in microwave irradiation. At a certain moment, the temperature dropped sharply from 110 degrees to 50 degrees, the reaction was still violent. Have you noticed a drop in temperature as carbon dioxide emission starts? View attachment 9888

w2x3f5buenas noches una pregunta de 1k bmk 5449-12-7. Relise con 1k fosforico. Baje al ph 3 purificado.
al final rindios. 200g polvo es normal o en q falle??

 

[w2x3f5]

buenas noches una pregunta de 1k bmk 5449-12-7. Relise con 1k fosforico. Baje al ph 3 purificado.
al final rindios. 200g polvo es normal o en q falle??

cernalit0000Puedes escribirme en inglés en mensajes privados

 

[btcboss2022]

this is the preparation of P2P Phenylacetone CAS 103-79-7 made use of BMK Glycidic Acid ( sodium salt ) CAS 5449-12-7 with main ingredient sulfonic acid strength is 75% CAS 7664-38-2
-------------------------------------------------- ------------------------------
we are going to prepare 1 kg of BMK
take a 5 liter double neck flask
add 500ml boiling water . start with the mixer.
now slowly add 1kg of BMK salt. then add 1 liter of sulfonic acid. now connect the reflux and heat the contents of the flask to max temperature. plus minus 130°c. use a powerful mixer
Let it boil in reflux for 4 hours.
take the top layer and pour it into a measuring cup.
let the bottom layer cool and save for next time. ( we have no chemical waste for this preparation method )

now boil 1 liter of water and add it to the measuring cup. use a hand mixer to mix everything.
After mixing for a few minutes, let the measuring cup cool to room temperature.
remove the top white layer (this is water and waste that we don't need)
the bottom layer is P2P purified and ready to use.

ps: in this preparation we don't have to worry about water remaining in our P2P because water weighs less than P2P

ps2: if you keep these ratios, the P2P will have a ph value of 4 .
if you use more sulfonic acid the ph value will drop to 1. Therefore it is not necessary to use too much sulfonic acid.

T0RWhy you talk about sulfonic acid when the CAS is phosphoric acid? Are different products.

 

[diogenes]

Why you talk about sulfonic acid when the CAS is phosphoric acid? Are different products.

btcboss2022I was just about to ask the same question. TOR are you using sulphonic or phosphonic (H3PO3) acid?

 

[merlin]

Introduction​

Hydrolysis of BMK glycidate ethers is represented in this topic. The procedure is the same for ethyl (Et) [cas 41232-97-7] and methyl (Me) [cas 80532-66-7] esters of glycidic acid. In case of sodium (Na) salt of this acid [cas 5449-12-7], you can skip first stage of NaOH addition and start from acid hydrolysis. In addition, purification method of obtained P2P is described. This procedure have to be committed to get pure Phenylacetone (P2P) for further syntheses of methamphetamine or amphetamine.

Suppliers of BMK glycidate ethers can be found in BB Listing.

Difficulty rating: 2/10 View attachment 6617 ​

Equipment and glassware:

• 1000 mL Round bottom flask;
• Reflux condenser;
• Retort stand and clamp for securing apparatus;
• pH indicator paper;
• Vacuum source (optional);
• Rotovap machine (optional);
• Glass rod and spatula;
• 100 mL x2; 250 mL x2; 500 mL x2 Beakers;
• Magnetic or top stirrer with a heating plate;
• Water bath;
• Funel;
• 1000 mL Separatory funnel;
• Vacuum distillation setup (optional);

Reagents:​

• 100 g BMK glycidate ethers (cas 80532-66-7; cas 41232-97-7; cas 5449-12-7);
• ~20 g NaOH or KOH;
• ~80 ml HCl (35%) or 100 ml H2SO4 (45%);
• ~600 mL DCM or Petroleum Ether;
• ~100 g MgSO4 or Na2SO4;
• ~500-600 mL Distilled water;
• ~ 50 g NaCl (optional);

View attachment 6616 ​

Hydrolysis of BMK glycidates​

1. NaOH (or KOH) 20g is dissolved in 250-300 ml distilled water with stirring. The reaction mixture (Rm) have to be cooled to room temperature. BMK glycidate 100 g (methyl or ethyl ester) is added and dissolved completely. Part of BMK is hydrolyzed during this procedure and floated as an oil in the surface of Rm. Rm is stired for 1 h at 75-80 °C with a reflux condenser.
2. Then, 200 ml HCl (35%) or 240 ml H2SO4 (45%) are added in small portions to Rm and heated to 80-90 °C and stired for 3 h. Rm have to be cooled to room temperature, the precipitate is filtered.
3. The reaction solution is extracted with DCM or petroleum ether 3 x 100 ml. Extract is washed with brine to neutral pH 7 several times. Extract is dried with MgSO4 (or Na2SO4) (optional) and filtered from solids.
4. An organic solvent (DCM or petroleum ether) is distilled off to give 65 ml of P2P.
​

P2P purification​

1. The resulting phenylacetone (P2P) is transferred to a round bottom flask with distilled water 1:1 (w/w) and distilled with steam under vacuum.
2. Purified P2P from receiver flask is extracted from water mixture with DCM (or petroleuum ether) 3 x 100 mL. Extract is dried with MgSO4 (or Na2SO4).
3. The resulting solution is filtered from the solids (drying agent) and then an organic solvent is distilled off.

Phenylacetone can be stored long time in a sealed vessel in a freezer. It is recommended to distill it before further syntheses of methamphetamine or amphetamine. Avoid direct sunlight onto phenylacetone and exposure to high temperature​

G.Patton
It would be good if we had one like this pmk to mdma

 

[adbb5clsupplier]

It would be good if we had one like this pmk to mdma

merlinsure,cas 28578-16-7

 

[diogenes]

Can anyone advice on which precursor is best to buy I mean safest to ship to Europe? Is any of the BMK powders legal - where can this be checked? I`m a bit confused as there are quite a few versions available.

 

[adbb5clsupplier]

Can anyone advice on which precursor is best to buy I mean safest to ship to Europe? Is any of the BMK powders legal - where can this be checked? I`m a bit confused as there are quite a few versions available.

diogenesBMK5449-12-7

 

[Smahk]

I am also having the same problem as @Costa. First batch I made came out fine.
2nd batch made with larger amount same ratio ,following the same instructions, also lumpy precipitate after cooling down past 30 degrees. Anyone know why? Thanks

 

[G.Patton]

I am also having the same problem as @Costa. First batch I made came out fine.
2nd batch made with larger amount same ratio ,following the same instructions, also lumpy precipitate after cooling down past 30 degrees. Anyone know why? Thanks

SmahkHi, I wrote my solution to @Costa but he didn't replied about his result. You can try my theory and reply here.

you can take the solid orange "p2p oil" from your beaker (take couple grams) and dissolve in water at room temperature or with slight heating (about 30 deg C). I think that this solid is water soluble salt. If you'll get oily layer on the top, I am right.

 

[Smahk]

Just wash your solid by distilled water to dissolve salts. You need DCM layer, bottom. DCM has 1.33 g/ml density, water has 1.0 g/ml.

G.PattonLooks like dcm went to top layer?

 

[G.Patton]

Looks like dcm went to top layer?

SmahkYes, looks like this. Probably water layer changed density by amount of salts.

 

[Smahk]

Yes, looks like this. Probably water layer changed density by amount of salts.

G.PattonThanks for help once again. Keep yellow bottom dcm layer still right?

 

[G.Patton]

Thanks for help once again. Keep yellow bottom dcm layer still right?

SmahkYou show pic with DCM top layer, now you telling me about bottom one. I'm a little messed up. Can you distinguish which layer is DCM and which is water by smell? Is there any problems?

 

[Smahk]

You show pic with DCM top layer, now you telling me about bottom one. I'm a little messed up. Can you distinguish which layer is DCM and which is water by smell? Is there any problems?

G.PattonThat’s why I’m confused. Dcm is more dense. So should be on bottom. But looks like dcm is on top and smells like dcm is on top right now. Thanks

 

[Botsauto-Dutchland]

That’s why I’m confused. Dcm is more dense. So should be on bottom. But looks like dcm is on top and smells like dcm is on top right now. Thanks

Smahkit can be on top if water is saturated with mixable or soluble salts or liquids. add more water 1/2 time the lower layer volume

 

[Botsauto-Dutchland]

That’s why I’m confused. Dcm is more dense. So should be on bottom. But looks like dcm is on top and smells like dcm is on top right now. Thanks

Smahkand if not sure keep both layers and heat them seperately

 

[edy's]

That’s why I’m confused. Dcm is more dense. So should be on bottom. But looks like dcm is on top and smells like dcm is on top right now. Thanks

SmahkDcm burns

 

[Botsauto-Dutchland]

Dcm burns

edyvanellendehow you let it burn ?

 

[edy's]

how you let it burn ?

Botsauto-DutchlandOkee.u are the first who woke up

 

[w2x3f5]

Small update on microwave synthesis. P2P from CAS 25547-51-7 (not sodium salt, sodium salt may require more acid). Mix 200 grams of CAS 25547-51-7 and 100 ml of phosphoric acid in a heat-resistant glass, add boiling stones. Irradiate in a microwave oven for a total around 20 minutes at a power of 1000 watts, with breaks for cooling. The reaction temperature is in the range of 50-120 degrees, the reaction starts at a temperature above 100 degrees, then due to the release of carbon dioxide, the temperature drops to 50-60 degrees - this is normal, towards the end of the synthesis the temperature rises to 120 degrees. The end of the reaction is determined by the cessation of carbon dioxide evolution. Final yield after P2P distillation 120 ml of clear colorless oil, less than 1 gram density per ml, or 80 percent of theory.

 

[w2x3f5]

Small update on microwave synthesis. P2P from CAS 25547-51-7 (not sodium salt, sodium salt may require more acid). Mix 200 grams of CAS 25547-51-7 and 100 ml of phosphoric acid in a heat-resistant glass, add boiling stones. Irradiate in a microwave oven for a total around 20 minutes at a power of 1000 watts, with breaks for cooling. The reaction temperature is in the range of 50-120 degrees, the reaction starts at a temperature above 100 degrees, then due to the release of carbon dioxide, the temperature drops to 50-60 degrees - this is normal, towards the end of the synthesis the temperature rises to 120 degrees. The end of the reaction is determined by the cessation of carbon dioxide evolution. Final yield after P2P distillation 120 ml of clear colorless oil, less than 1 gram density per ml, or 80 percent of theory.

w2x3f5I repeated this experiment, the output coincided, about 120 ml of oil, 80 percent of theory.

 

[mithyl2]

when using cas 5449-12-7, do i add the BMK to distilled water on it's own without naoh? is everything exactly the same as working with the other cas numbers except i just omit adding naoh to the water in the very first step?
not trying to ask a stupid question, just be specific.

and maybe cas 5449-12-7 isn't the best to work with due to the problems outlined by smahk and costa above.
is there a better one of the three cas numbers to use?

 

[w2x3f5]

Try hydrolysis in pure phosphoric acid in the microwave. I got a yield of 80% percent of the theoretical, p2p of good quality, the meth turned out to be excellent, now I am optimizing the synthesis of p2p on sodium borohydride.
Later I will publish the result of repeated synthesis in the microwave, it is important to obtain a stable repeating synthesis result.

 

[mithyl2]

Try hydrolysis in pure phosphoric acid in the microwave. I got a yield of 80% percent of the theoretical, p2p of good quality, the meth turned out to be excellent, now I am optimizing the synthesis of p2p on sodium borohydride.
Later I will publish the result of repeated synthesis in the microwave, it is important to obtain a stable repeating synthesis result.

w2x3f5does this work with 'cas 41232-97-7', 'cas 80532-66-7' or 'cas 5449-12-7'?

 

[w2x3f5]

does this work with 'cas 41232-97-7', 'cas 80532-66-7' or 'cas 5449-12-7'?

mithyl2Why not? I made sodium salt 5449-12-7, the yield is about the same.

 

[mithyl2]

Try hydrolysis in pure phosphoric acid in the microwave. I got a yield of 80% percent of the theoretical, p2p of good quality, the meth turned out to be excellent, now I am optimizing the synthesis of p2p on sodium borohydride.
Later I will publish the result of repeated synthesis in the microwave, it is important to obtain a stable repeating synthesis result.

w2x3f5thanks for letting us know. what's the best way to get pure phosphoric acid? it's a solid isn't it?