HRID411613

反应详情

EQUATION

反应方程式

HRID 411613 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2-[[[3-Methyl-4-(2,2,2-trifluoroethoxy)-2-pyridyl]methyl]sulfinyl]-1H-benzimidazole (370 mg) was dissolved in 20 ml of dichloromethane and 1 ml of triethylamine. Pyridine-3-sulfonyl chloride (195 mg) was added and stirred in ice-bath for 5 hr. Dichloromethane layer was washed with an aqueous solution composed of 0.1M NaCl and 0.1M sodium bicarbonate. Dichloromethane layer was dried over anhydrous magnesium sulfate. Solvent was removed under reduced pressure. Residual material was precipitated by dichloromethane-ethyl ether-heptane to provide 348 mg of 1-(pyridine-3-sulfonyl)-2-[(3-methyl-4-(2,2,2-trifluoroethoxy)-2-pyridyl)methylsulfinyl]-1H-benzimidazole.

WORKUP

后处理

  1. washDichloromethane layer was washed with an aqueous solution
  2. dry with materialDichloromethane layer was dried over anhydrous magnesium sulfate
  3. customSolvent was removed under reduced pressure
  4. customResidual material was precipitated by dichloromethane-ethyl ether-heptane