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.

 

[Win Win]

Hi sir… after reaction so i still need extracted by DCM and vaporrator?

 

[damakemi]

let the bottom layer cool and save for next time. ( we have no chemical waste for this preparation method )

what are the method on the second run using the bottom layer from the previous time?

 

[Win Win]

Hi sir. I am facing a difficult problem now, my p2p has turned milky white. Is there any way to save it? Can I use distilled water for washing?

 

[jessejames122669]

I got confused over the sulfonic acid part. I understand he was using phosphoric acid.
I now have sulfonic acid. Not phosphoric. Can sulfonic be used?
Anybody try it? Results?

 

[Jesse_Pinkman_]

All 3 acids (hci/phos/sulf) work, but there seems to different results in yield and different experiences. Every one has its one temp and time to convert and maybe prufication necessary.

 

[Win Win]

After reaction is it must extracted by dcm? And wash with brine?

 

[Saul]

@Win Win no you dont need dcm for this

 

[Saul]

@jessejames122669 yes son phosphoric acid I use very sorry, but we can change mistakes after 10 minutes
Very frustrating, I know .

 

[rothschild33]

After acquiring possible P2P from this reaction, would bisulfite adduct confirm that it is in fact P2P? or are there other ketones that could possibly result from the procedure?

 

[MisterAnonymous]

I used phosphoric acid and first the Rm went from light green to dark green after boiling for 3 hours 2 layers formed and i took the top layer but it's a very thick solution very tick is this P2P or something else?

 

[Saul]

looking verry good .
have you wash it with hot water ?

 

[MisterAnonymous]

No is it normal that it's so thick when i store it in the fridge it doesn't come out the bottle?

 

[Saul]

you need to wash it use mixer with hot water at least 3 liters and then give it 12hours

 

[Win Win]

Hi sir. I am facing a difficult problem now, my p2p has turned milky white. Is there any way to save it? Can I use distilled water for washing?

 

[G.Patton]

I don't know why it happened with your p2p. How do you store it? In an opened bottle under sun light? You can steam distill it, it should help to save part of this.

 

[Win Win]

I don't know why this happened, I sealed it and stored it in a cool place. Do I need to add distilled water for distillation? At what degree is the temperature controlled?

 

[G.Patton]

Watch video about d-meth manufacturing, there is video tutorial how to carry out steam distillation of P2P.

 

[Win Win]

Noted with thanks

 

[btcboss2022]

Is there any way to recover an "overcooked" bmk 5449? I didnt realize about that flask while doing other tasks , I tried the standard and logical ways without success.
Thanks.

 

[G.Patton]

Hi, I don't clearly understand your issue. Write me DM your problem, I'll try to help you.

 

[Win Win]

I
I use the method is 100g bmk add 100g distrilled water and 100g HCI after that heat up to 80c reflux 3 hour. Is it ok?