HRID657017

反应详情

EQUATION

反应方程式

HRID 657017 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To a solution of triphosgene (3.613 g, 12.175 mmol) in toluene (15 ml) was added a solution of 5-chloro-2-nitroaniline (2.100 g, 12.175 mmol) in toluene (15 ml) over 0.5 h and then the reaction was heated at 80° C. for 24 h. The reaction was then cooled and carefully poured onto aqueous NH3. This mixture was stirred for 1 h, filtered, washed with water (100 ml), MeOH (50 ml) and ethyl acetate (50 ml) to leave the desired product as a yellow solid (1.558 g, 60%).

WORKUP

后处理

  1. temperatureThe reaction was then cooled
  2. filtrationfiltered
  3. washwashed with water (100 ml), MeOH (50 ml) and ethyl acetate (50 ml)