HRID1596242
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customThe catalyst was removed by filtration through diatomaceous earth
- customthe solvent removed from the filtrate by evaporation
- customThe residue was purified by flash chromatography
- washeluting with methylene chloride/hexane (1/4)