P2P synthesis from BMK glycidate ethers

[G.Patton]

Do you use H3PO4 cons or diluted solution? Thank you for your feedback.

 

[microsharp]

same question， i used h3po4, 98% con, and get the p2p, but after i burn the p2p, it left white powder. but as i know, p2p, if burn, leave nothing

 

[G.Patton]

sorry, what did you burn? For what reason?

 

[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

 

[w2x3f5]

Have you tried water steaming the ketone from flask?

 

[w2x3f5]

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

 

[41Dxflatline]

I lied I didn't basify this time. Microwaved on low for 1:30 mins in 10 second intervals cooling and vigorous swirling between. Result: Nothing. I took it from the microwave and it's now sitting on a hotbed at 80C mildly "refluxing" (there's a small glass funnel with the hole stuffed sat on the flask) it's been about an hour and now its turned into cum with lots of tiny tiny bubbles throughout. It's still going and I'll leave it until there's a change.

 

[41Dxflatline]

Yield still not great but at least it looks decent:

 

[w2x3f5]

If the photo shows a mixture of glycidate and phosphoric acid, then your reaction is not known when it will pass, you have a separation of layers and hydrolysis will take forever without stirring. We need a homogeneous mixture, then the hydrolysis will go well

 

[diogenes]

Based on my results with sulphuric acid drain cleaner (instead of phosphoric acid which I didn`t have at the time), this is what I got in the receiving flask after the steam distillation. I figured this can only be P2P+water, the P2P separating as a separate layer in the distillate.

 

[w2x3f5]

but what yield?

 

[Lordoftheshard 2]

When you say to steam distilled the P2P are you adding lye to it or just steaming the P2P with no lyeI be using external steam distillation from a pressure cooker PTFE tubbing with a glass tube on the end of the PTFE tube the glass tube goes threw a rubber bung onto side neck in to the flask

 

[w2x3f5]

no lye is used, the steam itself perfectly captures the ketone. a big plus if you have superheated steam (temperature above 100 degrees), it captures the ketone better (the solubility of the ketone in the steam increases). When using a steam pipe, keep in mind that part of the steam is being cooled

 

[Lordoftheshard 2]

I tried steaming it it just released some powder that sat on top of the P2P so I poured of that the power and started again it just cleaning the P,,2,P in that flask it's not blowing it over as it should do I got some P2,P that came over but i expected a lot more than going to DCM extract all of the water

 

[w2x3f5]

If I understood you correctly, then the steam condensed in your flask with p2p, but it’s hard for me to understand what you did exactly.

 

[Lordoftheshard 2]

I put the P2P in the round bottom flasks 2,neck recovery Bend in neck attached to condenser side neck rubber stopper with a hole in the middle glass tube igies there there until the bowl my source if steam pressure cookers I use the to steam distill meth Fb
I put the glass tube that pumps the steam into the flask into the P2P it should really push ckeab FB and water over the recovery bend down the condenser into receiving flask I only got a tiny but if oil pushed over the rest was water. In the bowl I have this powdery substance mixed with water and a bug brown blob in the bottom also the oh if P2 po nwaa 2.5 I have done 20 Navi bribe washes I'd 25% to try raise the oh to 7= the oh haven't moved. Can J use the ph 2.5 p2p to make meth with btc synthesis medium scale methylaminre and sodium borohydride
Also when you do hydrolosisif bmk to P2P with phosphoric aacid .it's impossible to heat to 130celcuis with out burning the product I have a 10litreround bottom flask with 600mm Liebig condenser and when you go for 130vapour pressure is right at the too if the condenser 110us half way which I refluxed 6hours

 

[w2x3f5]

I didn’t understand anything, or my translator doesn’t work well, or you don’t write clearly. In addition to the fact that you make steam separately, although you can make steam directly in the reaction flask. 130 degrees for what are you trying to get? At 110 degrees, the reaction is excellent.

 

[Lordoftheshard 2]

So your saying you are adding water to the reaction mix and distilling it over I'm stead of using using a external source like U have used how much water do.yku add fir 1kg

 

[w2x3f5]

12 ml of water per 1 ml of ketone, this is with a margin. don't be lazy, I've written this many times on the forum.

 

[Ortist]

Most confusing thread I have ever read. So to summarize: It is better to use big excess of phosphoric acid and heat to 110 C to prevent incomplete reaction. Strong stirring is essential. Do we need to add some alcohol to the RM to prevent 2-phase formation?

 

[cartelloszetas]

Much more easy can made p2p form MEK

 

[Ortist]

i made it before via perborate route.
yelds however are low, workup is messy, requires a gas generator.
bayer-villager reaction tends to runaway at big loads and requires temperature control (too cold= solidifies, too hot = peracid fumes everywhere and boiling).
just wanted to try something new and glycidate salt seems easy to make.


PS: MEK route can be done without gas generator by using iPrOH or other suitable solvent with required amount of HCL dissolved in it. So you can measure exact amount of HCL needed without weighting your reaction flask every time.

 

[cartelloszetas]

Of cours bro if u are no chemist u cant made it

 

[Lordoftheshard 2]

Just follow the bmk and phosphoric acid route reflux @110c foours then let the reaction cool down separate the layers and steam distill the p2p cleans the p2p to nice yellow colour then use in which reaction you choose