HRID2120192

反应详情

EQUATION

反应方程式

HRID 2120192 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2.50 g (10 mmol) of 3,5-di-tert-butyl-4-hydroxy-benzoic acid are heated with 2.5 ml of thionyl chloride under reflux for 30 minutes. The reaction mixture is evaporated in vacuo and the residue is mixed with petroleum ether to remove the excess of thionyl chloride. 2.05 g (10 mmol) of compound obtained in Example 4 are mixed with 8.6 g of dry pyridine and dried ether. To this suspension there is added, dropwise, the ethereal solution of acyl chloride prepared above; the reaction mixture is refluxed for 30 minutes. The solvents are removed in vacuo. The residue is washed with water and dried. The title compound is crystallised from ethyl acetate.

WORKUP

后处理

  1. temperatureunder reflux for 30 minutes
  2. customThe reaction mixture is evaporated in vacuo
  3. additionthe residue is mixed with petroleum ether
  4. customto remove the excess of thionyl chloride
  5. additionTo this suspension there is added
  6. temperaturethe reaction mixture is refluxed for 30 minutes
  7. customThe solvents are removed in vacuo
  8. washThe residue is washed with water
  9. customdried
  10. customThe title compound is crystallised from ethyl acetate