HRID867538

反应详情

EQUATION

反应方程式

HRID 867538 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 15.2 g (50 mmol) of (S)-8-chloro-11,12,13,13a-tetrahydro-1-(hydroxymethyl)-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepin-9-one, 60 g of manganese (IV) oxide and 300 ml of methylene chloride is stirred at room temperature for 1.5 hours. The mixture is suction filtered over Dicalit, the residue is rinsed with methylene chloride and the filtrate is evaporated. After recrystallization from methylene chloride/ethyl acetate there is obtained (S)-8-chloro-11,12,13,13a-tetrahydro-9-oxo-9H-imidazo [1,5-a]pyrrolo[2,1-c][1,4]benzodiazepine-1-carboxaldehyde of melting point 224°-225°.

WORKUP

后处理

  1. filtrationfiltered over Dicalit
  2. washthe residue is rinsed with methylene chloride
  3. customthe filtrate is evaporated
  4. customAfter recrystallization from methylene chloride/ethyl acetate there