HRID895123

反应详情

EQUATION

反应方程式

HRID 895123 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Thiomorpholine (728 mg, 7.06 mmol) was added to a stirring solution of 3,4,5-trifluoronitro benzene (500 mg, 2.82 mmol) in acetonitrile (15 mL) and the reaction mixture was refluxed for 5 h. Evaporation of the solvent in a rotavapor under reduced pressure left a pasty mass which was dissolved in ethyl acetate (50 mL). Ethyl acetate portion was washed with water (30 mL×2) followed by brine (30 mL) and dried over sodium sulfate. Removal of volatiles yielded the title compound as yellow solid (650 mg, 85%).

WORKUP

后处理

  1. temperaturethe reaction mixture was refluxed for 5 h
  2. customEvaporation of the solvent in a rotavapor under reduced pressure
  3. waitleft a pasty mass which
  4. dissolutionwas dissolved in ethyl acetate (50 mL)
  5. washEthyl acetate portion was washed with water (30 mL×2)
  6. dry with materialdried over sodium sulfate
  7. customRemoval of volatiles