Large Scale APAAN Synthesis?
- Thread starter Blammo
- Start date
Well I've done the reaction a few times and always just followed the orgsyn procedure to a T which is written for roundabout 250g of benzyl cyanide which is more than I ever used in one go... sodium metal is not that easy to come by in large amounts and I stopped bothering with that route to P2P and went the PAA route from benzyl cyanide instead.
The hydrolysis of the nitrile to PAA is easy peasy and only requires H2SO4 while PAA to P2P can be done in pretty much any scale in pretty decent yields and rather easy setup and reagents. If you're looking for a solid batch process then PAA + GAA + FeSO4 in high boiling solvent is a very good method that works like a charm or in case you're looking for a continous process and industrial kind of prodiuction then the good ole tube furnace route with preferably a cobalt-manganese catalyst on a suitable support works very reliable.
The hydrolysis of the nitrile to PAA is easy peasy and only requires H2SO4 while PAA to P2P can be done in pretty much any scale in pretty decent yields and rather easy setup and reagents. If you're looking for a solid batch process then PAA + GAA + FeSO4 in high boiling solvent is a very good method that works like a charm or in case you're looking for a continous process and industrial kind of prodiuction then the good ole tube furnace route with preferably a cobalt-manganese catalyst on a suitable support works very reliable.
- By Blammo
You can buy sodium methoxide in powder form, skipping the need and some difficulty of procuring and using sodium.
I really appreciate the PAA plus GAA plus FeSO4, I have read that iron salts can be used, but now how. I assumed one would form the iron acetate, and the iron salts of phenylacetic acid
What are some high boiling solvents you would recommend? Just by Google, there is ethylene glycol. What temp would you recommend as well? I thought i read that iron salts could be used at reasonable temps, while calcium salts require very high temps.
If only the wilgerodt reaction of styrene to phenylacetic acid didn't need morpholine (somewhat hard to get in the US, fairly watched iirc) and produce hydrogen sulphide when hydrolysing the amide to the carboxylic acid.
I really appreciate the PAA plus GAA plus FeSO4, I have read that iron salts can be used, but now how. I assumed one would form the iron acetate, and the iron salts of phenylacetic acid
What are some high boiling solvents you would recommend? Just by Google, there is ethylene glycol. What temp would you recommend as well? I thought i read that iron salts could be used at reasonable temps, while calcium salts require very high temps.
If only the wilgerodt reaction of styrene to phenylacetic acid didn't need morpholine (somewhat hard to get in the US, fairly watched iirc) and produce hydrogen sulphide when hydrolysing the amide to the carboxylic acid.
How to make benzyl cyanide?the simplest way?