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
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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]

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?

 

[cernalit0000]

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??

 

[w2x3f5]

Puedes escribirme en inglés en mensajes privados

 

[btcboss2022]

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

 

[diogenes]

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

 

[merlin]

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

 

[adbb5clsupplier]

sure,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]

BMK5449-12-7

 

[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]

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

 

[Smahk]

Looks like dcm went to top layer?

 

[G.Patton]

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

 

[Smahk]

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

 

[G.Patton]

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?

 

[Smahk]

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

 

[Botsauto-Dutchland]

it 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]

and if not sure keep both layers and heat them seperately

 

[edy's]

Dcm burns

 

[Botsauto-Dutchland]

how you let it burn ?

 

[edy's]

Okee.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]

I 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]

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

 

[w2x3f5]

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

 

[mithyl2]

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