HRID362436

反应详情

EQUATION

反应方程式

HRID 362436 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 4,10-dihydro-5H-thieno[3,2-c][1]benzazepine and 700 mg of 4-[(2-methylbenzoyl)amino]benzoyl chloride is stirred in 30 ml of methylene chloride in the presence of 3 ml of triethylamine for 8 hours. The volatiles are removed in vacuo to give a residue which is partitioned between chloroform and water. The organic layer is dried (Na2SO4) 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 543 mg of the desired product. M+1=439.

WORKUP

后处理

  1. customThe volatiles are removed in vacuo
  2. customto give a residue which
  3. customis partitioned between chloroform and water
  4. dry with materialThe organic layer is dried (Na2SO4)
  5. customthe filtrate evaporated in vacuo
  6. customto give a residue which
  7. customis purified by column chromatography on silica gel by elution with 30% ethyl acetate-hexane