反应详情

温度

80 °C

In 80 ml of dimethylformamide was dissolved 4.0 g (22.0 mmol) of 4,5-dihydro-6-mercapto-1-methylpyrazolo[3,4-d]pyrimidin-4(1H)-one [Helv. Chim. Acta, 42, 349 (1959)], and 9.1 g (66 mmol) of potassium carbonate and 3.34 ml (32.9 mmol) of 1,3-dibromopropane were added to the solution, followed by stirring at 80° C. for 8 hours. After evaporation of the solvent, the residue was subjected to partition between chloroform and water, and the chloroform layer was concentrated to dryness under reduced pressure. The residue was subjected to silica gel column chromatography and eluted with chloroform-methanol (100:1) to give 1.87 g (38%) of Compound 44. The compound was recrystallized from ethanol for purification.

1. additionwere added to the solution
2. customAfter evaporation of the solvent
3. customto partition between chloroform and water
4. concentrationthe chloroform layer was concentrated to dryness under reduced pressure
5. washeluted with chloroform-methanol (100:1)