HRID1296404

反应详情

EQUATION

反应方程式

HRID 1296404 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirring suspension of 7-benzyl-8-bromo-3-methylxanthine (10.06 g, 30.0 mmol) in anhydrous dimethylsulfoxide was added sodium hydride (864 mg, 36.0 mmol). After stirring at room temperature for 30 min, (R)-5-acetoxy-1-chlorohexane (5.9 g, 33.0 mmol) was added. After stirring at 70-75° C. for 12 hours, the mixture was cooled to room temperature, quenched with water (600 ml) and stirred at room temperature for 4 hours. The precipitate was filtered to provide (R)-1-(5-acetoxyhexyl)-7-benzyl-8-bromo-3-methylxanthine (12.31 g, 86% yield) as a beige powder.

WORKUP

后处理

  1. stirringAfter stirring at 70-75° C. for 12 hours
  2. temperaturethe mixture was cooled to room temperature
  3. customquenched with water (600 ml)
  4. stirringstirred at room temperature for 4 hours
  5. filtrationThe precipitate was filtered