HRID482947

反应详情

EQUATION

反应方程式

HRID 482947 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3-Octadecyl-1-tritylglycerol (2.93 g) and 0.8 g of pyridine were dissolved in 10 ml of dichloromethane, and, under ice-cooling and stirring, 0.78 g of phenyl chlorocarbonate was added dropwise. The mixture was stirred under ice-cooling for 30 minutes and at room temperature for an hour, followed by addition of 20 ml of dichloromethane and water. The organic layer was separated, washed with aqueous sodium hydrogen carbonate and water, and dried. The solvent was then distilled off and 5 ml of morpholine was added to the residue. The mixture was allowed to stand at room temperature overnight and the morpholine was distilled off. The residue was recrystallized from n-hexane to give 2.7 g of the above-identified compound melting at 78°-79° C.

WORKUP

后处理

  1. temperatureunder ice-cooling
  2. stirringThe mixture was stirred under ice-
  3. customThe organic layer was separated
  4. washwashed with aqueous sodium hydrogen carbonate and water
  5. customdried
  6. distillationThe solvent was then distilled off
  7. addition5 ml of morpholine was added to the residue
  8. distillationthe morpholine was distilled off
  9. customThe residue was recrystallized from n-hexane