HRID1962380
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
A mixture of 5-bromo-1-fluoro-2-methyl-3-nitro-benzene (9.96 g) and iron powder (11.9 g) in ethanol (100 ml), water (20 ml) and concentrated hydrochloric acid (2 ml) was heated at reflux for one hour. After cooling, the reaction mixture was filtered through hyflo (calcined diatomaceous earth) and concentrated. The residue was purified by chromatography on silica gel (ethyl acetate/cyclohexane 1:9 to 1:4). Yield: 7.06 g of 5-bromo-3-fluoro-2-methyl-phenylamine as an oil.
WORKUP
后处理
- temperaturewas heated
- temperatureat reflux for one hour
- temperatureAfter cooling
- filtrationthe reaction mixture was filtered through hyflo (calcined diatomaceous earth)
- concentrationconcentrated
- customThe residue was purified by chromatography on silica gel (ethyl acetate/cyclohexane 1:9 to 1:4)