HRID1835703

反应详情

EQUATION

反应方程式

HRID 1835703 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. stirringAfter stirring for 5 hours at 70-80° C.
  2. customthe solvent was evaporated under reduced pressure
  3. additionThe residue was treated with saturated aqueous ammonium chloride solution (50 ml)
  4. extractionextracted with ethyl acetate (3×75 ml)
  5. washThe combined extracts were washed with saturated aqueous sodium chloride solution (30 ml)
  6. dry with materialdried over magnesium sulfate
  7. concentrationconcentrated under reduced pressure
  8. customThe solid was purified by recrystallization from ethanol