HRID238671

反应详情

EQUATION

反应方程式

HRID 238671 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 3-trifluoromethylpyrazole (5.0 g, 36 mmol), triethylamine (7.0 mL, 50 mmol) in dichloromethane (40 mL) was added dimethylsulfamoyl chloride (5.5 mL, 51 mmol), and the reaction mixture was heated at reflux for 2 days. The resulting mixture was cooled to ambient temperature and filtered through a pad of silica gel using dichloromethane as eluent. The filtrate was then concentrated under reduced pressure to give an amber residue. The resulting residue was dissolved in diethyl ether. The ether solution was washed with water, dried (MgSO4), and concentrated under reduced pressure to give 8.71 g of the title compound.

WORKUP

后处理

  1. temperaturethe reaction mixture was heated
  2. temperatureat reflux for 2 days
  3. filtrationfiltered through a pad of silica gel
  4. concentrationThe filtrate was then concentrated under reduced pressure
  5. customto give an amber residue
  6. washThe ether solution was washed with water
  7. dry with materialdried (MgSO4)
  8. concentrationconcentrated under reduced pressure