P2P synthesis from BMK glycidate ethers

[blackburn]

how come after hydrolysis with HCI in get clear yellow/dark oil on top liquid.

but after separating the oil from the HCI, and washing it with boiling water, the oil settles very thickly on the bottom and becomes cloudy almost like honey.

 

[w2x3f5]

Its glycidate just without sodium, standard problem and usually its happens because HCl not so good work

 

[G.Patton]

Hello, probably your problem is in a steam distillation?

 

[G.Patton]

Looks like a not well separated solution.

P.S. you can ask me in DM. I if for free. You don't need to pay.

 

[Heisenblack]

Thank you, I have sent the message, please respond

 

[blackburn]

So we now try the phosphoric 85%

Got same result, good oil after 5h reflux , but Took some sample and wash with hot Water and the oil sinks to the bottom and gett Little lighter, check pic on the right side. @G.Patton @Ra226

 

[blackburn]

 

[w2x3f5]

Today I received a short report on the hydrolysis of sodium glycidate from another user. He tried two of my options, in the first case he received 9.2 ml of p2p (after draining 8 ml, he may have lost part of p2p on the dryers) from 20 grams of glycidate and the second version of hydrolysis from 20 grams he received 12 ml of p2p (it is not known whether it is dry p2p or not ). Theoretical reaction yield 13.5 ml p2p ketone

 

[G.Patton]

are you sure that you has exactly BMK glycidate?

 

[G.Patton]

Congratulation. Did you post it here to promote your personal advice service or want to share your minds?

 

[w2x3f5]

The hydrolysis was carried out under my guidance and according to my method Heisenblack. I think he will publish the methodology later, after up scaling

 

[w2x3f5]

before publishing, need to check the repeatability

 

[Heisenblack]

Yes I will publish the methodology after running 50gr batch, the 12ml p2p from 20 gr sodium glycidate was dry

 

[G.Patton]

Nice to read this =) Thank you.

 

[G.Patton]

Actually, I have no Idea what is it. I've never tried phosphoric acid method with reflux.

 

[w2x3f5]

overheating is very likely, ketone oxidizes easily, additional side reactions possible

 

[blackburn]

Yes this is 5449-12-7 @G.Patton

@w2x3f5 okey well i have to try My way ...

Thanks to both

 

[w2x3f5]

write me in private messages, you can independently check the method, check the result. suddenly there will be pitfalls

 

[Re186]

I will try scale synthesis from benzaldehyde to BMK to P2P in about a week, I intend to reflux the sulfuric acid mentioned in the article provided by @G.Patton , at that time I will share my opinion and post the original Experimental data

 

[metux]

Can i use brown red color oil,for reduction?

 

[Heisenblack]

The brown red color oil is the unreacted glycidic acid, it would be best to steam distill the ketone then use in the next step

 

[Megido]

I mean then you have oil, but this oil 6 month old and becomes red color,. Do I need redistill for next step.