HRID2086687

反应详情

EQUATION

反应方程式

HRID 2086687 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. temperaturewas heated
  2. temperatureat reflux temperature for 1 hour
  3. temperatureAfter cooling
  4. filtrationinsolubles were filtered off by Celite, and volatiles
  5. customwere removed by evaporation
  6. dissolutionThe residue was redissolved in ethyl acetate (50 mL)
  7. washthe whole washed with water and brine
  8. dry with materialAfter dried over MgSO4 and concentration in vacuo
  9. washThe residue was washed with hexane