HRID2401488

反应详情

EQUATION

反应方程式

HRID 2401488 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A stirred solution of 4-chloro-5-nitro-1,2-phenylenediamine (2.0 g, 10.66 mmol) and CDI (2.59 g, 16 mmol) in anhydrous THF (50 mL) was heated to 85° C. for 4 h. The reaction was allowed to cool and the solvents were removed under reduced pressure. The resulting residue was washed with 2M aqueous hydrochloric acid and recrystallised from methanol to afford 5-chloro-6-nitro-1H-benzo[d]imidazol-2(3H)-one as a brown solid (1.9 g, 84%), which was taken through to the next step with no further purification.

WORKUP

后处理

  1. temperatureto cool
  2. customthe solvents were removed under reduced pressure
  3. washThe resulting residue was washed with 2M aqueous hydrochloric acid
  4. customrecrystallised from methanol