HRID66809

反应详情

EQUATION

反应方程式

HRID 66809 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

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.

WORKUP

后处理

  1. additionA mixture of 9.7 g
  2. temperatureit was cooled in an ice-bath
  3. additionTo the mixture was then added
  4. washit was washed successively with 1 N potassium carbonate, 1 N hydrochloric acid, water and saturated sodium chloride
  5. customThe resulting solution was dried
  6. customevaporated in vacuo
  7. customleaving 14.5 g