HRID1421231

反应详情

EQUATION

反应方程式

HRID 1421231 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. stirringthe mixture was stirred at 70-80° C. for 5 hours
  2. customAfter evaporation of the solvent under reduced pressure
  3. extractionextracted with ethyl acetate (3×75 ml)
  4. washThe combined extracts were washed with saturated aqueous sodium chloride solution (30 ml)
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrate
  7. customThe product was purified by recrystallization from ethanol