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
To a solution of N-hydroxysuccinimide ester of 3-hexadecanoyloxyoctadecanoic acid (7.5 g) prepared by the method of Example 8 (1) in dimethylformamide (200 ml) was added a solution of Nε -benzyloxycarbonyl-L-lysine (6.6 g) in 1N sodium hydroxide (23.6 ml) at room temperature. The mixture was stirred at ambient temperature for 3 hours. The precipitated solid was collected by filtration and the filtrate was concentrated under reduced pressure. The solid and the residue was combined. Then, the mixture was acidified with dilute hydrochloric acid and extracted with ethyl acetate. The organic layer was washed with water. The ethyl acetate solution was dried over magnesium sulfate, and then concentrated to give a residue which was dried up by high vacuum pump to afford powder of Nα -(3-hexadecanoyloxyoctadecanoyl)-Nε -benzyloxycarbonyl-L-lysine (8.5 g).
WORKUP
后处理
- filtrationThe precipitated solid was collected by filtration
- concentrationthe filtrate was concentrated under reduced pressure
- extractionextracted with ethyl acetate
- washThe organic layer was washed with water
- dry with materialThe ethyl acetate solution was dried over magnesium sulfate
- concentrationconcentrated
- customto give a residue which
- customwas dried up by high vacuum pump