反応 #95087

反応方程式

3-(2-nitrophenyl)propenoic acid

ethyl chloroformate

octylamine

triethylamine

→

title compound

N-Octyl-3-(2-Nitrophenyl)propenamide

溶媒

dichloromethane

dichloromethane

dichloromethane

反応条件

後処理

1. 1
   workup.ADDITIONA mixture of 9.7 g
2. 2
   温度it was cooled in an ice-bath
3. 3
   workup.ADDITIONTo the mixture was then added
4. 4
   洗浄it was washed successively with 1 N potassium carbonate, 1 N hydrochloric acid, water and saturated sodium chloride
5. 5
   その他The resulting solution was dried
6. 6
   その他evaporated in vacuo
7. 7
   その他leaving 14.5 g

実験手順

A mixture of 9.7 g. of 3-(2-nitrophenyl)propenoic acid, 5.6 g. of triethylamine and 240 ml. of dichloromethane was stirred at room temperature for 20 minutes, and then it was cooled in an ice-bath. To the mixture was then added, dropwise, during 15 minutes, a solution of 6.0 g. of ethyl chloroformate in 20 ml. of dichloromethane. After 15 minutes of stirring, a solution of 7.1 g. of octylamine in 20 ml. of dichloromethane was added dropwise, during 10 minutes. The reaction mixture was allowed to warm to room temperature, and then it was washed successively with 1 N potassium carbonate, 1 N hydrochloric acid, water and saturated sodium chloride. The resulting solution was dried and evaporated in vacuo, leaving 14.5 g. (95%) yield of the title compound as a tan solid.

出典