HRID1372653
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
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
- filtrationFrom the reaction mixture, the catalyst was filtered off
- distillationThe filtrate was distilled under reduced pressure
- customto remove the solvent
- customThe residue was purified by chromatography on a silica gel column, whereby from ethyl acetate/hexane (1/2) eluate fractions