HRID3554

反应详情

EQUATION

反应方程式

HRID 3554 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 5 mmol of 6,7-dihydro-5-(4-nitrobenzoyl)-5H-pyrrolo[1,2-a][1,5]benzodiazepine in 25 ml of ethyl alcohol is added 0.3 g of 10% Pd/C and 15 mmol of hydrazine followed by stirring and heating under reflux for 3 hours. The reaction mixture is filtered through diatomaceous earth. The filtrate is concentrated in vacuo to a residue which is dissolved in methylene chloride and passed through a pad of hydrous magnesium silicate. The filtrate is concentrated in vacuo to give the desired product which is purified by flash chromatography on silica gel to give the desired product as a solid.

WORKUP

后处理

  1. temperatureheating
  2. temperatureunder reflux for 3 hours
  3. filtrationThe reaction mixture is filtered through diatomaceous earth
  4. concentrationThe filtrate is concentrated in vacuo to a residue which
  5. dissolutionis dissolved in methylene chloride
  6. concentrationThe filtrate is concentrated in vacuo