反应详情

温度

60 °C

1.71 g (12.0 mmol) of potassium carbonate were added to a hot solution of 2.2 g (7.7 mmol) of 7-benzyl-3-propylxanthine from stage a) in 60 ml of dimethylformamide at 60° C. and the mixture was stirred at 60° C. for 1 hour. 0.93 ml (10.0 mmol) of ethoxymethyl chloride was then added dropwise and the mixture was stirred at 80° C. for 4.5 hours. A further 0.5 ml (5.3 mmol) of ethoxymethyl chloride was then added and the mixture was again stirred for 6 hours. 12 ml of water and 5 ml of methanol were then added, the mixture was allowed to stand overnight, 60 ml of water were added again and the mixture was extracted three times using methyl tert-butyl ether. The combined organic phases were washed twice with water, dried using magnesium sulfate and concentrated under reduced pressure. The crude product was purified by flash chromatography on a silica gel column, dichloromethane/methanol (19.8/0.2).

1. stirringthe mixture was stirred at 80° C. for 4.5 hours
2. stirringthe mixture was again stirred for 6 hours
3. waitto stand overnight
4. extractionthe mixture was extracted three times
5. washThe combined organic phases were washed twice with water
6. customdried
7. concentrationconcentrated under reduced pressure
8. customThe crude product was purified by flash chromatography on a silica gel column, dichloromethane/methanol (19.8/0.2)