反应详情

a mixture of 142 parts of N,N-dimethyl-2-hydroxyiminoacetoacetamide (a compound of Formula III), 1200 parts of toluene, 123 parts of p-anisidine and 1 part of p-toluenesulfonic acid was refluxed overnight in a flask fitted with a Dean-Stark distilling trap and water condenser. Eighteen parts of water were removed in this manner. On cooling, a heavy slurry of solid product precipitated. This was filtered and washed with butyl chloride thereby providing a product which melted at 201.5°-203° C. Recrystallization from acetonitrile gave 151 parts of N,N-dimethyl-2-hydroxyimino-3-(4-methoxyphenylimino)butyramide (a compound of Formula II) as a yellow solid, m.p. 204°-205.5° C.

1. temperaturewas refluxed overnight in a flask
2. customfitted with a Dean-Stark
3. distillationdistilling trap and water condenser
4. customEighteen parts of water were removed in this manner
5. temperatureOn cooling
6. customa heavy slurry of solid product precipitated
7. filtrationThis was filtered
8. washwashed with butyl chloride
9. customthereby providing a product which melted at 201.5°-203° C
10. customRecrystallization from acetonitrile