反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
In 200 ml of dried dichloromethane was dissolved 32.0 g (53.4 mmole) of 1-trityl-3-octadecylglycerol, and 22.4 ml of dried pyridine and then a solution of 6.7 ml (57.9 mmole) of benzoyl chloride in 100 ml of dried dichloromethane were added dropwise to the solution under stirring at 0° to 3° C. over the period of time of 30 minutes. The reaction mixture was stirred at room temperature for another 2 hours, and then concentrated under reduced pressure. 200 ml of ether was added to the residue, and the insoluble material was filtered off. The filtrate was concentrated, and the residue was purified by silica gel column chromatography (hexane:ethyl acetate=9:1) to give 28.8 g (7%) of 2-benzoyl-3-octadecyl-1-tritylglycerol as an oily material.
WORKUP
后处理
- stirringThe reaction mixture was stirred at room temperature for another 2 hours
- concentrationconcentrated under reduced pressure
- addition200 ml of ether was added to the residue
- filtrationthe insoluble material was filtered off
- concentrationThe filtrate was concentrated
- customthe residue was purified by silica gel column chromatography (hexane:ethyl acetate=9:1)