反应详情

A suspension of 100 kg of 4-methyl-3-oxo-N-phenylpentanamide (Example B) in 660 kg of hexanes is treated with agitation under nitrogen with 8 kg of β-alanine, 47 kg of benzaldehyde, and 13 kg of glacial acetic acid. The resulting suspension is heated to reflux with removal of water for 20 hours. An additional 396 kg of hexanes and 3 kg of glacial acetic acid is added and reflux continued with water removal for one hour. The reaction mixture is cooled to 20°-25° C. and the product is isolated by filtration. The product is purified by slurrying in hexanes at 50°-60° C., cooling, and filtration. The product is slurried twice with water at 20°-25° C., filtered, and dried in vacuo to yield 110 kg of 4-methyl-3-oxo-N-phenyl-2-(phenylmethylene)pentanamide, mp 143.7°-154.4° C.

1. temperatureThe resulting suspension is heated
2. temperaturereflux
3. customcontinued with water removal for one hour
4. temperatureThe reaction mixture is cooled to 20°-25° C.
5. customthe product is isolated by filtration
6. customThe product is purified
7. customby slurrying in hexanes at 50°-60° C.
8. temperaturecooling
9. filtrationfiltration
10. customis slurried twice with water at 20°-25° C.
11. filtrationfiltered
12. customdried in vacuo