HRID25498

反应详情

EQUATION

反应方程式

HRID 25498 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Dimethylformamide (25 mL) was added to 5,6-dichloro-2-(4-methoxy-3-nitro-phenyl)-1H-benzoimidazole (1.01 g, 3 mmol) from Step A. As the mixture stirred, sodium hydride (0.168 g, 4.2 mmol) was gradually added. After 3 hours, benzyl chloroformate (0.857 mL, 6 mmol) was added dropwise to the mixture. The reaction mixture was stirred overnight and then was partitioned between water (1,000 mL) and ethyl acetate (500 mL). The solvent was removed on the rotary evaporator and the residue triturated with 4:1 hexane:ethyl acetate to give the product (0.62 g), mp 212-214° C.

WORKUP

后处理

  1. stirringThe reaction mixture was stirred overnight
  2. customwas partitioned between water (1,000 mL) and ethyl acetate (500 mL)
  3. customThe solvent was removed on the rotary evaporator
  4. customthe residue triturated with 4:1 hexane