HRID1421231
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
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) at 70° C. and stirred for 1 hour. Benzyl bromide (1.2 ml) was added and the mixture was stirred at 70-80° C. for 5 hours. After evaporation of the solvent under reduced pressure, the residue was suspended in 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 concentrate. The product was purified by recrystallization from ethanol. Yield=1.06 g.
WORKUP
后处理
- stirringthe mixture was stirred at 70-80° C. for 5 hours
- customAfter evaporation of the solvent under reduced pressure
- 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
- concentrationconcentrate
- customThe product was purified by recrystallization from ethanol