HRID408695

反应详情

EQUATION

反应方程式

HRID 408695 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

To a mixture of 4,5-dichloro-2-nitro-phenylamine (1.29 g, 6.23 mmol) and dry MeOH (2 mL), a 25 wt % solution of sodium methoxide in MeOH (10 mL) was added and the mixture stirred for 6 h at 100° C. in a sealed tube. The mixture was cooled to 23° C., poured into water (50 mL), and extracted with EtOAc (3×50 mL). The combined organic layers were washed with brine (25 mL), dried, filtered, and concentrated under reduced pressure to afford the titled compound (0.700 g, 56%). The crude material was used without further purification in the next reaction.

WORKUP

后处理

  1. temperatureThe mixture was cooled to 23° C.
  2. extractionextracted with EtOAc (3×50 mL)
  3. washThe combined organic layers were washed with brine (25 mL)
  4. customdried
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure