HRID396800
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 4-(methylsulfonyl)-3-(trifluoromethyl)nitrobenzene (1.55 g, 5.76 mmol), iron powder (1.61 g, 28.8 mmol), and ammonium chloride (0.031 g, 0.58 mmol) in ethanol (30 mL), and water (8 mL) was heated at reflux temperature for 1 hour. After cooling, insolubles were filtered off by Celite, and volatiles were removed by evaporation. The residue was redissolved in ethyl acetate (50 mL) and the whole washed with water and brine. After dried over MgSO4 and concentration in vacuo. The residue was washed with hexane to give the subtitle compound (1.05 g, 76.2%, yield).
WORKUP
后处理
- temperaturewas heated
- temperatureat reflux temperature for 1 hour
- temperatureAfter cooling
- filtrationinsolubles were filtered off by Celite, and volatiles
- customwere removed by evaporation
- dissolutionThe residue was redissolved in ethyl acetate (50 mL)
- washthe whole washed with water and brine
- dry with materialAfter dried over MgSO4 and concentration in vacuo
- washThe residue was washed with hexane