HRID1276117

反应详情

EQUATION

反应方程式

HRID 1276117 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 3.52 g (88 mmol) of sodium hydroxide in 100 ml of methanol was slowly added dropwise to a mixture of 15.00 g (45 mmol) of methyl 2-chloro-3-(5-methyl-4,5-dihydroisoxazol-3-yl)-4-methylsulfonylbenzoate and 200 ml of methanol. The suspension was stirred at room temperature for 48 hours. The solvent was distilled off, the residue was taken up in water and the aqueous phase was washed three times with ethyl acetate. The aqueous phase was acidified with hydrochloric acid and extracted three times with ethyl acetate. The combined organic phases were subsequently washed neutral with water, dried and concentrated. 13.20 g (92% of theory) of 2-chloro-3-(5-methyl-4,5-dihydroisoxazol-3-yl)-4-methylsulfonylbenzoic acid were obtained.

WORKUP

后处理

  1. distillationThe solvent was distilled off
  2. washthe aqueous phase was washed three times with ethyl acetate
  3. extractionextracted three times with ethyl acetate
  4. customdried
  5. concentrationconcentrated