Three different Acetamide syntheses

[demorol]

Since acetamide is needed in Hoffmann synthesis of methylamine, I decided to collect all possible syntheses.

I. Acetamide from Acetyl chloride
In test tube put 2 mL of conc. NH3 solution and put it into ice-water bath. Drop by drop add 1 mL acetyl chloride. Add acetyl chloride slowly, so the white fumes that appear don't escape from the test tube. If precipitate does not form add some ether or ether/methanol mixture.

II. Acetamide from Acetanhydride
Put 2 mL of conc. NH3 solution into test tube and  put it in ice-water bath. Drop by drop add 1 mL of Acetanhydride. In this case white fumes don't appear. To this mixture add ether/methanol mixture until precipitate forms.

III. Acetamide from Ethyl acetate
Put 2 mL of conc. NH3 solution and 1 mL Ethyl acetate into test tube and shake it. When you can see only one layer add ether or ether/methanol mixture until precipitate forms.

First 2 synthesis I performed by myself. The third one was taken from all kind of sources and improved.
Give me some chemicals and I'll give you pleasure

[Rhodium]

And the yields from the various methods? For the first two, I suspect there are hydrolysis losses from reaction of the acetylation agents with water.

[PEYOTE]

Bubbling NH3 in the reagent should not provoke losses by hydrolisis, but maybe quite dangerous, doesn't it?

[Rhodium]

Not with a suck-back trap for the NH3 gas, and dilution of the acetylation reagent in an inert solvent.

[Osmium]

Ammonium acetate and heat. Why making it more complicated and expensive than it really is.

[Prdy2GO]

This is good info, Swim has a question say you already have plenty of acetamide and would like to rearange it to MeAm gas and their must be a better way than what strike describes in TSII. I am interested in in pratice technique not theroy. Swim uses the decompisition of hexamine mostly because it is so easy.
...
..
.

Hum did you get that?