HRID905081

反应详情

EQUATION

反应方程式

HRID 905081 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

9.77 g of benzoyl chloride were slowly added dropwise to a solution of 7.20 g of 2-hydroxymethyl-3,4-dihydro-2H-pyran in 14 ml of dry pyridine, whilst cooling the solution on an ice-water bath. When the addition was complete, the mixture was stirred at room temperature for 2 hours and then poured into an aqueous solution of sodium bicarbonate. The mixture was extracted with diethyl ether and the ethereal extract was washed with aqueous sodium chloride and dried over anhydrous sodium sulphate. The solvent was then evaporated off under reduced pressure and the residue was purified by distillation under reduced pressure, to give the title compound boiling at 112°-113° C./10 mmHG.

WORKUP

后处理

  1. temperaturewhilst cooling the solution on an ice-water bath
  2. additionWhen the addition
  3. extractionThe mixture was extracted with diethyl ether
  4. extractionthe ethereal extract
  5. washwas washed with aqueous sodium chloride
  6. dry with materialdried over anhydrous sodium sulphate
  7. customThe solvent was then evaporated off under reduced pressure
  8. distillationthe residue was purified by distillation under reduced pressure