反应详情

温度

70 °C

To a solution of 735 mg of 7-bromo-1-cyclopentyl-1,5-dihydro-4H-pyrazolo[4,3-c]quinolin-4-one in 6 mL of dimethylsulfoxide were sequentially added 49 mg of palladium acetate, 91 mg of 1,3-bis(diphenylphosphino)propane, 0.62 mL of triethylamine, and 3 mL of methanol, and the atmosphere in the reaction container was replaced with carbon monoxide. The mixture was stirred at 70° C. for 7 hours, cooled to room temperature, and then poured into a mixture of water and ethyl acetate. The aqueous layer was separated, the organic layer was washed with diluted hydrochloric acid and saturated brine, and then dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography (chloroform/methanol) to obtain 551 mg of methyl 1-cyclopentyl-4-oxo-4,5-dihydro-1H-pyrazolo[4,3-c]quinoline-7-carboxylate.

1. temperaturecooled to room temperature
2. customThe aqueous layer was separated
3. washthe organic layer was washed with diluted hydrochloric acid and saturated brine
4. dry with materialdried over anhydrous magnesium sulfate
5. customthe solvent was evaporated under reduced pressure
6. customThe obtained residue was purified by silica gel column chromatography (chloroform/methanol)