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
CONDITIONS
反应条件
- 温度
- 70 °C
PROCEDURE
实验过程
A solution of sodium hydroxide (400 mg) in water (5 ml) was added to a suspension of 3,8-dimethylxanthine (1.80 g) in methanol (10 ml). After stirring for 1 hour at 70° C., benzyl bromide (1.2 ml) was added. After stirring for 5 hours at 70-80° C., the solvent was evaporated under reduced pressure. The residue was treated with saturated aqueous ammonium chloride solution (50 ml) and extracted with ethyl acetate (3×75 ml). The combined extracts were washed with saturated aqueous sodium chloride solution (30 ml), dried over magnesium sulfate and concentrated under reduced pressure. The solid was purified by recrystallization from ethanol to provide 7-benzyl-3,8-dimethylxanthine (1.06 g).
WORKUP
后处理
- stirringAfter stirring for 5 hours at 70-80° C.
- customthe solvent was evaporated under reduced pressure
- additionThe residue was treated with saturated aqueous ammonium chloride solution (50 ml)
- extractionextracted with ethyl acetate (3×75 ml)
- washThe combined extracts were washed with saturated aqueous sodium chloride solution (30 ml)
- dry with materialdried over magnesium sulfate
- concentrationconcentrated under reduced pressure
- customThe solid was purified by recrystallization from ethanol