HRID2116679

反应详情

EQUATION

反应方程式

HRID 2116679 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
130 °C

PROCEDURE

实验过程

51.0 g (158 mmol) (E)-2-acetylamino-3-(4-amino-3-chloro-5-trifluoromethyl-phenyl)-acrylic acid, dissolved in 408 ml NMP, were combined with 612 ml aqueous 4-molar hydrochloric acid solution and stirred for 3 hours at a bath temperature of 130° C. stirred. The reaction mixture was cooled and poured onto 2000 ml of water with stirring. The precipitate formed was suction filtered, washed with 400 ml of water, dried overnight at 60° C. and recrystallised from 1000 ml boiling toluene.

WORKUP

后处理

  1. stirringstirred
  2. temperatureThe reaction mixture was cooled
  3. stirringwith stirring
  4. customThe precipitate formed
  5. filtrationfiltered
  6. washwashed with 400 ml of water
  7. customdried overnight at 60° C.
  8. customrecrystallised from 1000 ml