HRID889484

反应详情

EQUATION

反应方程式

HRID 889484 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

Ethyl phenylmethyl (2-fluoro-4-nitrophenyl)propanedioate (3.86 g, 10.6 mmol) dissolved in ethanol (50 ml), was treated with ammonium formate (6.7 g, 10.6 mmol) under argon. Palladium on carbon 10% paste (380 mg) was added and the reaction was stirred under reflux for 3 hours (60° C.). The reaction was cooled to room temperature and the catalyst removed by filtration through celite. Solvent was removed to give a brown oil. The crude material was purified by chromatography on silica gel eluting with 0-50% ethyl acetate in hexane (1:1) over 45 minutes. Fractions were evaporated to give the title compound as a yellow oil (1.26 g, 6.4 mmol).

WORKUP

后处理

  1. temperatureThe reaction was cooled to room temperature
  2. customthe catalyst removed by filtration through celite
  3. customSolvent was removed
  4. customto give a brown oil
  5. customThe crude material was purified by chromatography on silica gel eluting with 0-50% ethyl acetate in hexane (1:1) over 45 minutes
  6. customFractions were evaporated