HRID901606

反应详情

EQUATION

反应方程式

HRID 901606 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 3-(chlorosulfonyl)benzoic acid (2.00 g) and dichloromethane (20 ml) under nitrogen at 0° was treated with cyclohexylamine (3.63 ml) and the mixture was stirred at 0° for 0.5 h. The solvent was evaporated in vacuo and the residue was treated with 1M potassium hydrogen sulfate solution (50 ml) and extracted with EtOAc (3×50 ml). The combined extracts were dried (Na2SO4) and the solvent evaporated in vacuo to give the title compound (2.28 g). LCMS RT=3.16 min, ES+ve 284 (MH)+.

WORKUP

后处理

  1. customThe solvent was evaporated in vacuo
  2. additionthe residue was treated with 1M potassium hydrogen sulfate solution (50 ml)
  3. extractionextracted with EtOAc (3×50 ml)
  4. dry with materialThe combined extracts were dried (Na2SO4)
  5. customthe solvent evaporated in vacuo