HRID1962380

反应详情

EQUATION

反应方程式

HRID 1962380 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

A mixture of 5-bromo-1-fluoro-2-methyl-3-nitro-benzene (9.96 g) and iron powder (11.9 g) in ethanol (100 ml), water (20 ml) and concentrated hydrochloric acid (2 ml) was heated at reflux for one hour. After cooling, the reaction mixture was filtered through hyflo (calcined diatomaceous earth) and concentrated. The residue was purified by chromatography on silica gel (ethyl acetate/cyclohexane 1:9 to 1:4). Yield: 7.06 g of 5-bromo-3-fluoro-2-methyl-phenylamine as an oil.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux for one hour
  3. temperatureAfter cooling
  4. filtrationthe reaction mixture was filtered through hyflo (calcined diatomaceous earth)
  5. concentrationconcentrated
  6. customThe residue was purified by chromatography on silica gel (ethyl acetate/cyclohexane 1:9 to 1:4)