HRID2303843

反应详情

EQUATION

反应方程式

HRID 2303843 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 5.91 g of 2-chloro-3,5-dimethylbenzene-1,4-diol, 8.13 g of pyridine and 30 ml of dichloromethane, 10 ml of a dichloromethane solution containing 4.54 g of pivaloyl chloride were added dropwise under ice cooling, followed by stirring at the same temperature for one hour and at room temperature for 90 minutes. The reaction mixture was concentrated by evaporation. Water was added to the concentrate and the mixture was extracted with ethyl acetate. The extract was dried over anhydrous sodium sulfate and the solvent was distilled off under reduced pressure. The residue was purified by chromatography through a silica gel column (eluting solvent: n-hexane/ethyl acetate=10/1), whereby 8.02 g of the title compound were obtained.

WORKUP

后处理

  1. additionwere added dropwise under ice cooling
  2. concentrationThe reaction mixture was concentrated by evaporation
  3. additionWater was added to the
  4. concentrationconcentrate
  5. extractionthe mixture was extracted with ethyl acetate
  6. dry with materialThe extract was dried over anhydrous sodium sulfate
  7. distillationthe solvent was distilled off under reduced pressure
  8. customThe residue was purified by chromatography through a silica gel column (eluting solvent: n-hexane/ethyl acetate=10/1)