HRID399936

反应详情

EQUATION

反应方程式

HRID 399936 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 3.0 g (12 mmol) of 2-chloro-3-fluoro-4-methylsulfonylbenzoic acid in 15 mL of 3-methylpiperidine was heated at 70° C. with stirring for 6 days. The reaction mixture was diluted with aqueous hydrochloric acid and extracted with dichloromethane. The organic extract was dried over magnesium sulfate and the solvent was removed by concentration under reduced pressure. The residue obtained was crystallized from acetonitrile to obtain 2.4 g (60 percent of theory) of the title compound as a solid.

WORKUP

后处理

  1. extractionextracted with dichloromethane
  2. extractionThe organic extract
  3. dry with materialwas dried over magnesium sulfate
  4. customthe solvent was removed by concentration under reduced pressure
  5. customThe residue obtained
  6. customwas crystallized from acetonitrile