HRID428592

反应详情

EQUATION

反应方程式

HRID 428592 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

A mixture of methyl 3-fluoro-4-nitrobenzoate(2.14 g, 10.8 mmol) and iron powder(2.63 g) in acetic acid(22 ml) was stirred at 50° C. for 2.5 h. After cooling down to room temperature, CH2Cl2(100 ml) and water(300 ml) was added to the mixture and filtered to remove iron powder. The organic layer was separated and the aqueous layer was extracted with CH2Cl2(70 mlx2). The CH2Cl2 solution was combined, washed with water, brine, dried(Na2SO4), and concentrated to give 1.77 g(97%) of pale brown solid.

WORKUP

后处理

  1. temperatureAfter cooling down to room temperature
  2. filtrationfiltered
  3. customto remove iron powder
  4. customThe organic layer was separated
  5. extractionthe aqueous layer was extracted with CH2Cl2(70 mlx2)
  6. washwashed with water, brine, dried(Na2SO4)
  7. concentrationconcentrated