HRID2166441

反应详情

EQUATION

反应方程式

HRID 2166441 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A mixture of 3-[6-(triphenylmethoxy)hexyloxy]-2-metylenepropane-1-ol (from Preparation 46) (1.5 g) and pyridine (4.5 ml) in methylene chloride (15 ml) was cooled in an ice/water bath and octadecyloxycarbonyl chloride (1.3 g) was added. After stirring for 10 minutes at 0° C. the temperature was raised to 22° C. for 5 hours. Ether (15 ml) was added, and the mixture was filtered. The filtrate was evaporated to dryness in vacuo, and the residue was purified through a column of silica gel 60 (70-230 mesh, 15 g) eluting with ether/methylene chloride 1:1. Further purification was achieved by chromatography on Waters PrepLC®/System 500A using a prepPAK®-500/SILICA cartridge with ether/methylene chloride/pentane 1:1:3 as eluent.

WORKUP

后处理

  1. temperaturewas cooled in an ice/water bath
  2. temperaturewas raised to 22° C. for 5 hours
  3. filtrationthe mixture was filtered
  4. customThe filtrate was evaporated to dryness in vacuo
  5. customthe residue was purified through a column of silica gel 60 (70-230 mesh, 15 g)
  6. washeluting with ether/methylene chloride 1:1
  7. customFurther purification