HRID1792480

反应详情

EQUATION

反应方程式

HRID 1792480 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

200 mg ethyl 2-fluoro-4-(2-nitrophenylamino)benzoate (compound in Production Example 331), 180 mg iron powder, 350 mg ammonium chloride and 8 mL solution mixture of methanol and water (5:3) were stirred at 100° C. for 1 hour. Insolubles were filtered off with Celite, and water was added to the filtrate which was then extracted with dichloromethane. The extract was purified by NH silica gel chromatography (ethyl acetate), to give 179 mg of the title compound as pale brown crystals.

WORKUP

后处理

  1. filtrationInsolubles were filtered off with Celite, and water
  2. additionwas added to the filtrate which
  3. extractionwas then extracted with dichloromethane
  4. customThe extract was purified by NH silica gel chromatography (ethyl acetate)