反应详情

A suspension of 100 kg of 4-methyl-3-oxo-N-phenyl-pentanamide (Example A) in 660 kg of hexane was 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 was heated to reflux with removal of water for 20 hours. An additional 396 kg of hexane and 3 kg of glacial acetic acid was added and reflux continued with water removal for 1 hour. The reaction mixture was cooled to 20° C. to 25° C., and the product was isolated by filtration. The product was purified by slurring in hexane at 50° C. to 60° C., cooling, and filtrating. The product was slurred twice with water at 20° C. to 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. VPC: 30 meter DB-5 capillary column 50° C. to 270° C. at 15° C./min; 19.33 minutes, 99.7% (area). GC/MS: M/Z 293 [M]+.

1. temperatureThe resulting suspension was heated
2. temperaturereflux
3. customcontinued with water removal for 1 hour
4. temperatureThe reaction mixture was cooled to 20° C. to 25° C.
5. customthe product was isolated by filtration
6. customThe product was purified
7. customby slurring in hexane at 50° C. to 60° C.
8. temperaturecooling
9. filtrationfiltrating
10. customwas slurred twice with water at 20° C. to 25° C.
11. filtrationfiltered
12. customdried in vacuo