反应详情

To a suspension of sodium hydride (94 mg) in dimethoxyethane (10 ml) was added ethyl diethylphosphonoacetate (528 mg) and the mixture was stirred at room temperature for 15 minutes. Under ice-cooling, 4-(2-chlorophenyl)-5-cyano-6-formyl-4,7-dihydro-2H-pyrazolo[3,4-b]pyridine (670 mg) was added to the mixture, and the mixture was stirred at the same temperature for 1 hour. Water was added to the reaction mixture and the mixture was extracted with ethyl acetate. The extract was washed with a saturated aqueous sodium chloride solution and dried over anhydrous magnesium sulfate. The solvent was evaporated and the obtained residue was purified by silica gel column chromatography (eluent:hexane-ethyl acetate (1:1)) to give the title compound (560 mg) as yellow crystals.

1. temperatureUnder ice-cooling
2. stirringthe mixture was stirred at the same temperature for 1 hour
3. extractionthe mixture was extracted with ethyl acetate
4. washThe extract was washed with a saturated aqueous sodium chloride solution
5. dry with materialdried over anhydrous magnesium sulfate
6. customThe solvent was evaporated
7. customthe obtained residue was purified by silica gel column chromatography (eluent:hexane-ethyl acetate (1:1))