HRID323863

反应详情

EQUATION

反应方程式

HRID 323863 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.45 g (3.26 mmol) of potassium carbonate was added at 60° C. to a suspension of 0.65 g (2.04 mmol) of 7-benzyl-3-phenylxanthine from stage a) in 20 ml of dimethylformamide and the mixture was stirred at this temperature for one hour. 0.29 ml (2.65 mmol) of propoxymethyl chloride was then added dropwise and the mixture was stirred at 80° C. for 1.5 hours. 20 ml of water were then added, the mixture was extracted three times using 24 ml of methyl tert-butyl ether each time, and the combined organic phases were washed twice with 12 ml of water each time, dried using magnesium sulfate and concentrated under reduced pressure. The crude product was purified by flash chromatography on a silica gel column heptane/ethyl acetate (5/7).

WORKUP

后处理

  1. stirringthe mixture was stirred at 80° C. for 1.5 hours
  2. extractionthe mixture was extracted three times
  3. washthe combined organic phases were washed twice with 12 ml of water each time
  4. customdried
  5. concentrationconcentrated under reduced pressure
  6. customThe crude product was purified by flash chromatography on a silica gel column heptane/ethyl acetate (5/7)