HRID1956341
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
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
- customThe reaction mixture is evaporated in vacuo to a residue which
- extractionis extracted with chloroform
- washwashed with water
- dry with materialdried over Na2SO4
- filtrationfiltered
- customthe filtrate evaporated in vacuo
- customto give a residue which
- customis purified by column chromatography on silica gel by elution with 30% ethyl acetate-hexane