HRID1596242

反应详情

EQUATION

反应方程式

HRID 1596242 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

4-Chloro-5-methoxycarbonyloxy-2-fluoronitrobenzene (1.2 g, 4.8 mmol), (as described in EP 61741 A2), and 10% palladium-on-charcoal catalyst (500 mg) in ethanol (100 ml) was stirred under hydrogen at 1 atmosphere pressure for 18 hours. A further batch of 10% palladium-on-charcoal catalyst (500 mg) was added and the mixture stirred under hydrogen for a further 3 hours. The catalyst was removed by filtration through diatomaceous earth and the solvent removed from the filtrate by evaporation. The residue was purified by flash chromatography eluting with methylene chloride/hexane (1/4) to give 2-fluoro-5-methoxycarbonyloxyaniline (0.42 g, 47%) as an oil.

WORKUP

后处理

  1. customThe catalyst was removed by filtration through diatomaceous earth
  2. customthe solvent removed from the filtrate by evaporation
  3. customThe residue was purified by flash chromatography
  4. washeluting with methylene chloride/hexane (1/4)