HRID1675576

反应详情

EQUATION

反应方程式

HRID 1675576 的结构方程式

PROCEDURE

实验过程

To 100 ml of methanol were added 7.0 g of 4-benzyloxy-3,5-difluorobenzonitrile and 15 ml of concentrated sulfuric acid, and the resulting mixture was heated under reflux for 5 days. Thereafter, water was added to the reaction mixture which had been allowed to cool to near room temperature, followed by extraction with ethyl acetate. The organic layer was dried over magnesium sulfate, and concentrated under reduced pressure. The residue was subjected to silica gel column chromatography, and 4.5 g of methyl 3,5-difluoro-4-hydroxybenzoate was obtained.

WORKUP

后处理

  1. temperaturethe resulting mixture was heated
  2. temperatureunder reflux for 5 days
  3. extractionfollowed by extraction with ethyl acetate
  4. dry with materialThe organic layer was dried over magnesium sulfate
  5. concentrationconcentrated under reduced pressure