反应详情

A 500 mL, round-bottomed flask under a positive pressure of nitrogen was equipped with a magnetic stirrer and charged with absolute ethanol (90 mL) followed by N-{4-[4-(diethylcarbamoyl-phenyl-methyl)-piperazin-1-yl]-3-fluoro-phenyl}-2-pyridin-3-yl-benzamide (4.5 g, 7.9 mmol). 2M HCl in anhydrous ether (7.9 mL, 15.9 mmol) was added drop-wise to the reaction mixture via an addition funnel and the resulting suspension was stirred at ambient temperature for 2 h. The reaction mixture was diluted by the addition of anhydrous ether (90 mL) in a slow stream, which resulted in a gummy solid. The solvents were removed on the rotary evaporator to yield a pale brown foam. The foam was triturated with a mixture of dichloromethane/ether (45 mL each) and the resulting suspension was stirred at ambient temperature for 3 h, then at 0° C. for 1 h. The resulting solid was collected by filtration and the filter-cake was washed with 1:1 dichloromethane/ether (2×40 mL) and dried under house vacuum. The powder was dried further on the rotary evaporator (water bath temperature 50° C.) to yield the title compound as an off-while solid.

1. customA 500 mL, round-bottomed flask under a positive pressure of nitrogen was equipped with a magnetic stirrer
2. customresulted in a gummy solid
3. customThe solvents were removed on the rotary evaporator
4. customto yield a pale brown foam
5. customThe foam was triturated with a mixture of dichloromethane/ether (45 mL each)
6. stirringthe resulting suspension was stirred at ambient temperature for 3 h
7. waitat 0° C. for 1 h
8. filtrationThe resulting solid was collected by filtration
9. washthe filter-cake was washed with 1:1 dichloromethane/ether (2×40 mL)
10. customdried under house vacuum
11. dry with materialThe powder was dried further on the rotary evaporator (water bath temperature 50° C.)