HRID376410

反应详情

EQUATION

反应方程式

HRID 376410 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In 120 ml of xylene was dissolved 3.22 g (10 mmol) of 1-O-tritylglycerol, followed by addition of 3.36 g (30 mmol) of t-butoxypotassium under argon. After 5 minutes of stirring, 30 ml of a solution of 12.8 g (30 mmol) oleyl p-toluenesulfonate in xylene was added dropwise and the mixture was stirred under reduced pressure (20-30 mmHg) at ambient temperature for 30 minutes and, then, at 50 for 1 hour. The reaction mixture was then poured in ice-water and extracted with ether, and the extract was washed with water, dried, and concentrated. The residue was purified by column chromatography silica gel/n-hexane-ethyl acetate) to provide 6.10 g (73%) of 1,2-O-dioleyl-3-O-tritylglycerol.

WORKUP

后处理

  1. stirringthe mixture was stirred under reduced pressure (20-30 mmHg) at ambient temperature for 30 minutes
  2. waitat 50 for 1 hour
  3. extractionextracted with ether
  4. washthe extract was washed with water
  5. customdried
  6. concentrationconcentrated
  7. customThe residue was purified by column chromatography silica gel/n-hexane-ethyl acetate)