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 (S)-3-[(2S,3R,4R,5S)-2,3,4,6-tetrahydroxy-5-(L-leucyl)aminohexanoyl]amino-3-phenylpropionic acid hydrochloride (1.84 g) in methanol (40 ml) was added a solution of diphenyldiazomethane (1.45 g) in methanol (20 ml) and the mixture was stirred at room temperature for 4 hours. After addition of acetic acid (0.1 ml), the reaction mixture was extracted with ethyl acetate. The extract was washed with aqueous sodium hydrogencarbonate solution and saturated brine respectively and the ethyl acetate solution was dried over anhydrous sodium sulfate. Removal of the organic solvent gave a residue, which was purified by silica gel column chromatography. Elution with ethyl acetate-methnaol (2:1) provided the title compound (2.05 g).
WORKUP
后处理
- extractionthe reaction mixture was extracted with ethyl acetate
- washThe extract was washed with aqueous sodium hydrogencarbonate solution and saturated brine respectively
- dry with materialthe ethyl acetate solution was dried over anhydrous sodium sulfate
- customRemoval of the organic solvent
- customgave a residue, which
- customwas purified by silica gel column chromatography
- washElution with ethyl acetate-methnaol (2:1)