HRID1372653

反应详情

EQUATION

反应方程式

HRID 1372653 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Ethyl 3-fluoro-4-nitro-5-benzyloxyphenylacetate (1.54 g, 4.62 mmol) and 10% palladium-carbon (122 mg) were subjected to catalytic hydrogenation for 20 hours under normal pressure while stirring at room temperature in EtOH (20 ml). From the reaction mixture, the catalyst was filtered off. The filtrate was distilled under reduced pressure to remove the solvent. The residue was purified by chromatography on a silica gel column, whereby from ethyl acetate/hexane (1/2) eluate fractions, ethyl 4-amino-3-fluoro-5-hydroxyphenylacetate (639 mg, 65%) was obtained as a brown oil.

WORKUP

后处理

  1. filtrationFrom the reaction mixture, the catalyst was filtered off
  2. distillationThe filtrate was distilled under reduced pressure
  3. customto remove the solvent
  4. customThe residue was purified by chromatography on a silica gel column, whereby from ethyl acetate/hexane (1/2) eluate fractions