HRID323852

反应详情

EQUATION

反应方程式

HRID 323852 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

2.2 g (15.9 mmol) of potassium carbonate were added to a hot solution of 3 g (11.0 mmol) of 7-benzyl-3-cyclopropylxanthine from stage a) in dimethylformamide at 60° C. and the mixture was stirred at 60° C. for one hour. 1.51 g (15.9 mmol) of 2-methoxyethyl chloride were then added dropwise and the mixture was stirred at 80° C. for 6 hours. It was then allowed to cool to room temperature and concentrated under reduced pressure. The oily residue was taken up in dichloromethane and extracted using 1 N sodium hydroxide solution, washed with water until neutral, dried over magnesium sulfate and concentrated under reduced pressure, and the residue was employed in stage c) without further purification.

WORKUP

后处理

  1. stirringthe mixture was stirred at 80° C. for 6 hours
  2. temperatureto cool to room temperature
  3. concentrationconcentrated under reduced pressure
  4. extractionextracted
  5. washwashed with water until neutral,
  6. dry with materialdried over magnesium sulfate
  7. concentrationconcentrated under reduced pressure
  8. customwithout further purification