HRID1264625

反应详情

EQUATION

反应方程式

HRID 1264625 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

5

PROCEDURE

实验过程

Methyl 4-fluoro-3-nitrophenylacetate (5.0 g, 0.023 mol) and iron powder (3 g, 0.053 mol) were suspended in a mixture of propan-2-ol (50 ml) and water (5 ml). Concentrated hydrochloric acid (5 drops) was added at room temperature and the mixture was heated at reflux with stirring for 2 hours. The reaction mixture was cooled, diluted with diethyl ether, filtered through diatomaceous earth and the resulting filtrate was evaporated in vacuo. The residue was further purified by chromatography on silica gel, eluting with diethyl ether to yield methyl 3-amino-4-fluorophenylacetate (3.5 g) as a yellow oil.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureat reflux
  3. temperatureThe reaction mixture was cooled
  4. filtrationfiltered through diatomaceous earth
  5. customthe resulting filtrate was evaporated in vacuo
  6. customThe residue was further purified by chromatography on silica gel
  7. washeluting with diethyl ether