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.

 

[edy's]

So you figured it out now? Nice

 

[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?

 

[Costa]

Hi, as said, I repeated the process following the instructions of the document (and your comments) step by step. I got exactly the same product on this step:

I took the oily layer (top layer, which has P2P) and once it cooled down after 10 minutes it has this aspect:

.

Then I added DCM over the other layer (the "water") in order to make the first extraction, however, this was the aspect of the mixture:

as you can see, there was some kind of white precipitate on the bottom, there were not two layers, just the white solids and the rest.
What did I do wrong? The document is not very clear...
Many thanks in advance and sorry for that many questions, but this process it is being a headache...

 

[G.Patton]

It is quite strange. Check cas 5449-12-7 mp. Also, 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.

 

[UWe9o12jkied91d]

@Costa
What acid did you use?
Maybe if it’s sodium hydrogen sulphate, I don’t know how readily the acid reacts with dcm to form this but it’s am idea

 

[Saul]

@Costa
You did allot wrong my friend.
You use a single neck flask . it is not gonna work !
you need an powerful overhead mixer ( one neck )
you need reflux ( one neck )
you need to check temp ( one neck )
you can fix this with this

http://bbzzzsvqcrqtki6umym6itiixfhni37ybtt7mkbjyxn2pgllzxf2qgyd.onion/attachments/w718mivfez-jpg.9471/?hash=be1d7fb1cfef713907490cf27be3e967

 

[Benz88]

would a normal magnetic stirrer with heat function also go ? Instead overhead stirrer

 

[UWe9o12jkied91d]

yes

 

[Saul]

@Costa

1kg Bmk Salt = 700ml P2P

you dont need DCM
You dont need Steam Distillation
You need H2o for purifying and some time ( 24h ) to seperate the final product p2p

 

[Heisenblack]

Should it be pure distilled water or brine solution?

 

[Saul]

@Benz88

NO
you really need a powerful mixer so it is terror in the flask.
normal color is dark green not white when mixing 4 hours

magnetic is only good for very Small size

 

[Botsauto-Dutchland]

top layer dark green ? oke i did not had any terror in the flask it was outside the flask but what contruction used for top stirring or bought one ?

 

[Botsauto-Dutchland]

oke i ordered cas 5449-12-7
3L flask 600grams not sure it should be a kilo, 400gr left
its not a perfect situation! far from
i prepared all in a car 600gr into the flask. dont ask how long it took.
then 350 ml boiling water added and started heating, dropped 800ml of Phosforic acid in a few portions and put up the flame for 4 hours.
stirred with custom made magnetic stirrer until one hits my head taped it back on they died 3 hours later. then i put a huge 1kg powermeter magnet on it and i slowly stirred/shaked last hour.

i told the mans home owner that the smell should be accaptable.
It wasnt i bubbled true a basic ice cold solution, had a leak at custom made ball joint cone adapter. (so beunhaze sjit) Taped with extreme repair silicon tape but still smell lots of that effected my thoughts.
so after 4 hours it did not get over 125-130C i stopped i had a deep purple upper layer a white boddem layer you could see true.
I cleaned up and sepated the top layer i should not had done @ that temperature the smell was a apaan explosion. my car is runed by the smell
anyway day after into the woods a stainles steel bottel 2 flames 1 below one sideways steam is escaping a the end of my fast setup into the snow....

I left with some still white solution with a wite oil swimming on the bottem. I also did the half amount extracting with ether but this ended up the fire i made because of my sanity that cameback with the fresh air i was breathing wtf are i am doing ????
my feet that hurt so much i needed the flame trower for my feet so i gave up!
i will do it someday in a place its ''safe'' never @ my home i still cant acces. and i advice to use a mask with this cas i felt like i was missing the half of my braincells
so not that much of usefull information but i gues you do add the water after the acid (or not phosporic acid 75) you can reach higher temperatures or heat it mush longer. (ps i added Naoh before i steam distilled) and my next try with those 400gr will be with sulfuric acid and phosporic acid.

and one intrested in the smelly milk after steaming i give it for free (ex shipping) but i dont think its worth it.

 

[Saul]

@Botsauto-Dutchland

no bottom layer is green and top layer is yellow
and after cleaning the top layer with H2o you have a white and a yellow layer
after 24h the yellow layer is your p2p

 

[Saul]

@btcboss2022

T0R Why you talk about sulfonic acid when the CAS is phosphoric acid? Are different products.

ok my mistake sorry no normal replay or edit possible

phosphoric acid work best with bmk salt . very good yields

 

[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]

Thanks @G.Patton Will try this. And if it proves to be water soluble salt. How to move forward?
And another question. Next, Extraction of the water layer with DCM, do I keep top or bottom? Thanks!

 

[G.Patton]

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.

 

[UWe9o12jkied91d]

I extracted with solvent while it was still warm and had good yield and no solids.I guess you have to separate right after it has cooled a bit from heat

 

[Smahk]

After adding DCM it “looks” like DCM is on top with some oil. Which makes me think twice perhaps I did something wrong. Because the bottom layer colour looks like the original water colour.

 

[Botsauto-Dutchland]

how you let it burn ?

 

[edy's]

Okee.u are the first who woke up

 

[UWe9o12jkied91d]

Dcm will sink, just extract the non aqeous phase wherever it is, it’s not hard to tell
@Smahk