反应详情

温度

60 °C

2.1 g (15.2 mmol) of potassium carbonate were added to a hot solution of 3 g (10.0 mmol) of 7-benzyl-3-butylxanthine from stage a) in 90 ml of dimethylformamide at 60° C. and the mixture was stirred at 60° C. for one hour. 1.3 g (12.0 mol) of 3-methoxypropyl chloride were then added dropwise and the mixture was stirred at 100° C. for 3 hours. It was then allowed to cool to room temperature, and was treated with water and extracted using dichloromethane. The organic phase was washed with water and 1 N sodium hydroxide solution, dried using sodium sulfate and concentrated under reduced pressure. The oily residue was purified by flash chromatography on a silica gel column, toluene/ethanol (39/1)

1. stirringthe mixture was stirred at 100° C. for 3 hours
2. temperatureto cool to room temperature
3. extractionextracted
4. washThe organic phase was washed with water and 1 N sodium hydroxide solution
5. customdried
6. concentrationconcentrated under reduced pressure
7. customThe oily residue was purified by flash chromatography on a silica gel column, toluene/ethanol (39/1)