反应详情

温度

60 °C

2.12 g (15.3 mmol) of potassium carbonate were added to a solution of 2.0 g (9.6 mmol) of 3-methyl-7-propylxanthine in 60 ml of dimethylformamide at 60° C. and the mixture was stirred at 60° C. for one hour. Then 3.07 g (12.5 mmol) of 1-chloro-8-diethylamino-5-hydroxy-5-methyl-6-octyne from stage A1) were added dropwise and the mixture was stirred at 80° C. for 12.5 hours. It was then allowed to cool to room temperature, water was added, and three extractions with tert-butyl methyl ether were carried out. The organic phase was dried over magnesium sulfate, concentrated under reduced pressure and purified by flash chromatography, dichloromethane/methanol=19/1.

1. stirringthe mixture was stirred at 80° C. for 12.5 hours
2. temperatureto cool to room temperature
3. extractionthree extractions with tert-butyl methyl ether
4. dry with materialThe organic phase was dried over magnesium sulfate
5. concentrationconcentrated under reduced pressure
6. custompurified by flash chromatography, dichloromethane/methanol=19/1