HRID1276124

反应详情

EQUATION

反应方程式

HRID 1276124 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

9.80 g (75 mmol) of chlorocarbonylsulfenyl chloride were added dropwise to a solution of 4.37 g (15 mmol) of methyl 3-aminocarbonyl-2-chloro-4-methylsulfonylbenzoate in 150 ml of dry toluene. The mixture was stirred under reflux for 48 hours, and the solvent was then removed under reduced pressure and the residue was chromatographed over silica gel (eluent: ethyl acetate/cyclohexane=1/1). 3.70 g (70% of theory) of methyl 2-chloro-3-(1,3,4-oxathiazolin-2-on-5-yl)-4-methylsulfonylbenzoate were obtained.

WORKUP

后处理

  1. temperatureunder reflux for 48 hours
  2. customthe solvent was then removed under reduced pressure
  3. customthe residue was chromatographed over silica gel (eluent: ethyl acetate/cyclohexane=1/1)