HRID440730

反应详情

EQUATION

反应方程式

HRID 440730 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of 1.8 g of 10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine and 3 ml of triethylamine in 100 ml of methylene chloride at 0° C. is added a solution of 2.8 g of 4-iodobenzoyl chloride in 25 ml of methylene chloride. The reaction mixture is stirred at room temperature for 4 hours and evaporated in vacuo to a residue which is partitioned between water and chloroform. The organic layer is dried over Na2SO4, filtered and evaporated in vacuo to a brown residue which is crystallized from ether-hexane to give 3.0 g of the desired product. Mass spectrum: M+H:323.

WORKUP

后处理

  1. customevaporated in vacuo to a residue which
  2. customis partitioned between water and chloroform
  3. dry with materialThe organic layer is dried over Na2SO4
  4. filtrationfiltered
  5. customevaporated in vacuo to a brown residue which
  6. customis crystallized from ether-hexane