MAPA powder CAS 16648-44-5 conversion to P2P (1kg scale)

[btcboss2022]

Conversion:

1. 1kg of MAPA (Methyl 2-phenylacetoacetate) powder is dissolved in 1 liter of hot H2O with stirring
2. 3 Liters of HCL 37% are added
3. Reflux with stirring around 7-8 hours at 80-90C until the oily part seems brown.
4. Cooled in an Ice bath.
5. Now are 2 layers in the flask, separate and keep the bottom layer and extract twice with Ether or DCM.
6. Add the extractions to the first top layer and add 4 times it's volume in H2O to the mixture and stir.
7. The mixture is steam distilled, in first part of distillation the ether will comes out once ether finished change the receiver flask to start to receive the H2O+P2P(ether is discarded) distill until you see no more oily water came out or P2P smells disappears from the outgoing oily water.
8. Let it cool to room temperature and you will see the P2P layer on the bottom.
9. Separate layers, in this point you can decide to try to extract more from the water layer or not depends how clean you see the water.
10. P2P could be turbid about water depends of future use you can dry it with MgSO4.

680ml of P2P obtained.

 

[Saul]

I don't get it why this topic had so many views.
you have find yourself a legal way to create p2p.
this is great.

I will definitely try it too.
I'm just going to make some adjustments.
i use sulfuric acid 96% CAS 7664-93-9
So I need much less water.

 

[btcboss2022]

Hello,

You must take in account that CAS 16648-44-5 is not easy to obtain now but this method would work similar in new CAS of BMK powder I will confirm it very soon if something change but will be small changes for sure.
Thanks.

 

[Saul]

can you plz say what glass we needed for 1 kg pouder

 

[G.Patton]

10 L RB flask or Erlenmeyer flask;
Reflux condenser;
Ice bath;
Aquarium pump with a hose or a large preparatory funnel for ~5L;
Steam distillation setup (see Lab FAQ);
2-5 L Erlenmeyer flask;

 

[G.Patton]

Hello, do you know that it isn't BMK? It is Methyl 2-phenylacetoacetate (MAPA). Did you make mistake in the CAS of your substance or you carried out your synthesis from MAPA?

 

[btcboss2022]

Hello,

I know this CAS is MAPA but I though that people will understand better BMK powder than MAPA and the final goal is P2P anyway. I made this synth from MAPA yes.
Thankis

 

[G.Patton]

These are different substances and the title of the topic is misleading, I'll change it.

 

[Germanium]

 

[Germanium]

How is MAPA synthesised?

 

[G.Patton]

Procedure is the same with MeOH.

 

[Dope Amine]

Howdy folks. I've got a liter of mapa that I'm excited to convert to p2p. I need a little more info about this reaction if someone can kindly help out.

What are the byproducts of this reaction? Methanol and carbon dioxide?

Why is it necessary to use 36 moles of acid for 5.2 moles of MAPA? I'd love to reduce the volume by using diluted sulfuric acid (if that works well). Would it still require 36 moles of sulfuric, or could it bee reduced to 18 moles since H2SO4 is diprotic, or would 10 moles of sulfuric acid bee enough?

Many thanks

 

[btcboss2022]

A liter of MAPA? It should be powder until I know.

 

[Dope Amine]

Sorry, I meant to say a kilo. Yes, it is a powder, not a liquid.