P2P synthesis from BMK glycidate ethers

[Andrzej]

Yesterday I have tried the method with the microwave and in fact the result is interesting.
In baker mixed 20g 5449-12-7 and 20mL of 85% orto-phosphoric acid.
I put in microwave oven (700W), and set the lowest power. 5 -7 seconds of heating and 10-15 seconds brake for mixing and cooling the mixture because the temperature was too high. In sum 1 minute of active heating.
After heating added 50mL of distilled water.
Than extracted with dietyl ether (3x20mL) and washed with brine (3x100mL).
Dried with magnesium sulphate and evaporated ether:

Obtained very good looking product but only 7g from 20g of powder.
I was try again and heat in microwave longer - 2 minutes but there was no difference - the same yield (I was afraid of overheating because too much heat in microwave result creating solid, transparent glass-like surface which is unable to remove from baker).
Is there any method to improve the yield in microwave? Because now it is still between 30-40%?

 

[41Dxflatline]

I did this yesterday, got almost exactly the same result. One thing I did observe though is when I didn't mix it straight away it seemed more p2p was forming but upon mixing it didn't return to the surface. Some sort of emulsification with the lower layer or a misobservation on my part?

 

[w2x3f5]

are you confusing glycidate oil with p2p oil? =)

 

[41Dxflatline]

I don't know. There's only ever been 2 layers, a cloudy white bottom layer and a light yellow layer on top. There has never been any brown anything like in other photos. It's possible the p2p isn't p2p since I'm not familar with p2p and I've not tested it in any way. What is glycidate oil? Glycidic acid?

 

[w2x3f5]

pictured above is melted glycidate acid (not salt)

 

[41Dxflatline]

I'm pretty sure he took that photo at room temperature.

 

[w2x3f5]

To be precise, there is a mixture of p2p and glycidic acid, for this reason it does not crystallize at room temperature

 

[edy's]

Question here,i have a lot of phosphoric acid 75% can i just destill it to 85% or should that fuck my acid up?

 

[41Dxflatline]

First attempt in the microwave got me a low yield as reported. I tried a 2nd attempt.

40g 5449-12-7 and 40ml phosphoric acid were placed into a 250ml erlenmeyer flash and allowed to react while stirring. After CO2 production stopped the flask was then placed into a 800W microwave on the lowest setting for 1 minute, removed and stirred. Once settled it was returned to the microwave for another minute, stirred and returned again for a final 2 minutes. Absolutely no separation this time and the RM has acquired a slight flesh tone tint. Smells heavily of P2P though

View attachment 3uofqpMhAN.jpg

I'm going to pour in some brine

 

[edy's]

How dit it turn out?

 

[edy's]

Im trying same prod.but its a bitch.had a message from my vendor,from a custumer shes got and im going to give that a try.but have a strange feeling of the route .1.1 bmk 1kg water 1kg naoh and 1kg hcl .stir at roomtemp for 2hr .then stirr at 90C for 3 hr and then stop mixing.brown oil can be used directly for nex step. I will try soon but am not so shure about first step and the hcl part .but maby try to swich that with phosforic acid.didnt test it yet but came straight from the vendor and she/he never let me down tho.for products delivery shes one of a kind.so im tended to think it will be profitable.but im puzzeled about it by the info i got here to so .... il let you know how it turned out if you like

 

[41Dxflatline]

Separated, still shit yield. Even worse than before

 

[w2x3f5]

Have you tried water steaming the ketone from flask?

 

[41Dxflatline]

No. lab here or glassware. Just 2 erlenmeyers,

 

[w2x3f5]

How did you isolate the ketone?

 

[41Dxflatline]

I havent gone that far, it either separates into layers on its own (Attempt 1) or does so if you add some brine and a little more salt

 

[w2x3f5]

there may be a mixture of ketone and glycidic acid, cleaning is needed.

 

[edy's]

Talking CAS 5449 12 7

 

[edy's]

Man this shit is though getting it richt.or am i the only one having a hard time getting it it up over the 65%? Beare with me im aving an ego drop here from not getting it up and working like im used to.feel so bad working with it.but heard that IF you got it richt it is one of the most high yealding powders.but those are storys no confermation on any colegas

 

[edy's]

Shit keeps me awake for weeks now.im in need of some good yealds by now

 

[edy's]

But for what i heard.it should all be done at low temp.like in the range of 90C.im puzzelend here .i get it to make verry clean oil but getting a good stable yealding route above 65% is a real chalange

 

[41Dxflatline]

Gonna basify next time