反応 #54987

反応方程式

N,N-dimethyl-2-hydroxyiminoacetoacetamide

p-anisidine

p-toluenesulfonic acid

→

N,N-dimethyl-2-hydroxyimino-3-(4-methoxyphenylimino)butyramide

溶媒

toluene

反応条件

後処理

1. 1
   温度was refluxed overnight in a flask
2. 2
   その他fitted with a Dean-Stark
3. 3
   workup.DISTILLATIONdistilling trap and water condenser
4. 4
   その他Eighteen parts of water were removed in this manner
5. 5
   温度On cooling
6. 6
   その他a heavy slurry of solid product precipitated
7. 7
   ろ過This was filtered
8. 8
   洗浄washed with butyl chloride
9. 9
   その他thereby providing a product which melted at 201.5°-203° C
10. 10
    その他Recrystallization from acetonitrile

実験手順

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.

出典