HRID274451

反应详情

EQUATION

反应方程式

HRID 274451 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 1.49 g of 2-phenylethylamine in 100 ml of methylene chloride is treated with 1.26 g of triethylamine. A solution of 3.0 g of 3,4-dimethoxy-5-nitrobenzoyl chloride in 100 ml of methylene chloride is added dropwise thereto while stirring, whereupon the mixture is stirred for a further 15 minutes. The organic phase is then extracted twice with 50 ml of ice-water each time, dried over sodium sulfate and evaporated in a water-jet vacuum. After recrystallization from methylene chloride/n-hexane there is obtained 3,4-dimethoxy-5-nitro-N-phenethylbenzamide in the form of pale beige needles of m.p. 121°-122°.

WORKUP

后处理

  1. stirringis stirred for a further 15 minutes
  2. extractionThe organic phase is then extracted twice with 50 ml of ice-water each time
  3. dry with materialdried over sodium sulfate
  4. customevaporated in a water-jet vacuum
  5. customAfter recrystallization from methylene chloride/n-hexane there