反应详情

To a solution of 3-(4-{2-[5-(4-acetylpiperazin-1-yl)pyridin-2-yl]ethyl}thiophen-2-yl)propan-1-ol (150.0 mg, 0.402 mmol) in anhydrous tetrahydrofuran (3 ml) was added 1,1′-carbonyldiimidazole (84.7 mg, 0.522 mmol), and the mixture was stirred at room temperature for 2 hrs. 1M Hydrazine tetrahydrofuran solution (1.21 ml, 1.21 mmol) was added, and the mixture was stirred at room temperature for 2 hrs. Since the reaction did not proceed, hydrazine monohydrate (26.1 mg, 0.522 mmol) was added, and the mixture was stirred at room temperature for 1 hr. The reaction mixture was concentrated under reduced pressure, and the residue was purified by aminopropylated silica gel column chromatography (5%-2-propanol-dichloromethane mixture) and aminopropylated silica gel column chromatography (2%-methanol-dichloromethane mixture) to give the title compound (148.8 mg, yield 85.9%) as a colorless syrup.

1. stirringthe mixture was stirred at room temperature for 2 hrs
2. stirringthe mixture was stirred at room temperature for 1 hr
3. concentrationThe reaction mixture was concentrated under reduced pressure
4. customthe residue was purified by aminopropylated silica gel column chromatography (5%-2-propanol-dichloromethane mixture) and aminopropylated silica gel column chromatography (2%-methanol-dichloromethane mixture)