HRID1265926

反应详情

EQUATION

反应方程式

HRID 1265926 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A mixture of 4-(3-bromoacetyl-phenyl)-8-chloro-7-dimethylamino-1,3-dihydro-benzo[b][1,4]diazepin-2-one (130 mg) (Example 193a) and N-amidino-thiourea (35 mg) in THF (3 mL) was heated at 60° C. for 1 h. The mixture was diluted with AcOEt and washed with sat. NaHCO3 solution and with brine. The organic layer was dried and evaporated and the residue was purified by chromatography on silica gel using AcOEt/MeOH (20:1) as eluent. The purified product was crystallyzed from acetone to give the title compound (22 mg) as yellow solid.

WORKUP

后处理

  1. washwashed with sat. NaHCO3 solution and with brine
  2. customThe organic layer was dried
  3. customevaporated
  4. customthe residue was purified by chromatography on silica gel