HRID1956341

反应详情

EQUATION

反应方程式

HRID 1956341 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 400 mg of 10,11-dihydro-10-[4-(2-thienyl)benzoyl]-5H-pyrrolo[2,1-c][1,4]benzodiazepine, 10 ml of 40% formalin and 10 ml of 40% N,N-dimethylamine in 50 ml of 1:1 tetrahydrofuran:methyl alcohol is refluxed for 3 hours. The reaction mixture is evaporated in vacuo to a residue which is extracted with chloroform, washed with water, dried over Na2SO4, filtered and the filtrate evaporated in vacuo to give a residue which is purified by column chromatography on silica gel by elution with 30% ethyl acetate-hexane to give 300 mg of the desired product as a solid. Mass spectrum: M+H:428.

WORKUP

后处理

  1. customThe reaction mixture is evaporated in vacuo to a residue which
  2. extractionis extracted with chloroform
  3. washwashed with water
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. customthe filtrate evaporated in vacuo
  7. customto give a residue which
  8. customis purified by column chromatography on silica gel by elution with 30% ethyl acetate-hexane