HRID1378163

反应详情

EQUATION

反应方程式

HRID 1378163 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

21.8 g (57.9 mmol) of ethyl (S)-8-bromo-9-oxo-12,12a-dihydro-9H,11H-azeto [2,1-c]imidazo [1,5-a][1,4]benzodiazepine-1-carboxylate were heated to reflux for 15 minutes with 17 ml of 4N sodium hydroxide solution and 200 ml of ethanol. 17 ml of 4N hydrochloric acid and 250 ml of water were added at room temperature. The alcohol was evaporated and the suspension was cooled to 0°. By suction filtration and drying the crystals there were obtained 19.8 g (98%) of (S)-8-bromo-9-oxo-12,12a-dihydro-9H,11H-azeto[2,1-c]imidazo[1,5-a][1,4]-benzodiazepine-1-carboxylic acid of m.p. 178°-180°.

WORKUP

后处理

  1. customThe alcohol was evaporated
  2. temperaturethe suspension was cooled to 0°
  3. filtrationBy suction filtration
  4. customdrying the crystals