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 stirring solution of (R)-3-(5-acetoxyhexyl)-1,7-dimethylxanthine (0.28 g, 0.87 mmol) in methanol (20 ml) was added an anhydrous solution of hydrogen chloride in ethyl ether (1 M, 2.6 ml, 2.6 mmol). After refluxing for 4 hours, the mixture was concentrated under reduced pressure. The residue was treated with saturated aqueous solution of sodium bicarbonate solution (30 ml) and extracted with dichloromethane (3×20 ml). The combined extracts were washed with saturated aqueous sodium chloride solution (30 ml), dried over sodium sulfate and concentrated under reduced pressure to give (R)-3-(5-hydroxyhexyl)-1,7-dimethylxanthine (0.20 g, 85% yield) as a colorless oil that solidified on standing.
WORKUP
后处理
- temperatureAfter refluxing for 4 hours
- concentrationthe mixture was concentrated under reduced pressure
- additionThe residue was treated with saturated aqueous solution of sodium bicarbonate solution (30 ml)
- extractionextracted with dichloromethane (3×20 ml)
- washThe combined extracts were washed with saturated aqueous sodium chloride solution (30 ml)
- dry with materialdried over sodium sulfate
- concentrationconcentrated under reduced pressure