反应详情

50 mg (0.23 mmol, 1.5 equiv.) of diphosphorus pentasulfide are added to a solution of 50 mg (0.15 mmol) of 6-(3-chlorobenzyl)-1-cyclopentyl-1,5-dihydro-4H-pyrazolo[3,4-d]pyrimidin-4-one (Example 1) in 1 ml of pyridine at room temperature, and the mixture is then stirred under reflux overnight. After cooling, the reaction solution is mixed with 10 ml of ice-cold 2.5% strength sodium bicarbonate solution and extracted three times with ethyl acetate. The combined organic phases are washed with saturated brine, dried over sodium sulfate and concentrated in vacuo. The crude product is purified by preparative HPLC.

1. temperatureunder reflux overnight
2. temperatureAfter cooling
3. extractionextracted three times with ethyl acetate
4. washThe combined organic phases are washed with saturated brine
5. dry with materialdried over sodium sulfate
6. concentrationconcentrated in vacuo
7. customThe crude product is purified by preparative HPLC