HRID80410

反应详情

EQUATION

反应方程式

HRID 80410 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of (2-trifluoromethylsulfanyl-ethanesulfonyl)-acetonitrile (190 mg, 0.81 mmol), trifluoro-methanesulfonic acid 2-trifluoromethylsulfanyl-ethyl ester (340 mg, 1.22 mmol) and K2CO3 (340 mg, 2.44 mmol) in 1,2-dimethoxyethane (10 mL) was stirred under nitrogen at room temperature overnight. The reaction mixture was diluted with H2O (40 mL) and extracted with ethyl acetate (3×30 mL). The combined organic extracts were washed with saturated aqueous NaCl solution, dried over Na2SO4 and concentrated under reduced pressure. The residue was purified by flash column chromatography (SiO2, gradient of EtOAc/cyclohexane) to afford compound II-26 (20 mg, 7%).

WORKUP

后处理

  1. extractionextracted with ethyl acetate (3×30 mL)
  2. washThe combined organic extracts were washed with saturated aqueous NaCl solution
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was purified by flash column chromatography (SiO2, gradient of EtOAc/cyclohexane)
  6. customto afford compound