反应详情

N-tert-Butyl-3((4-(4-nitrobenzoyl)piperazin-1-yl)methyl)benzamide (0.56 g, 1.31 mmol) was dissolved In methanol (10 mL) at room temperature. Raney 2800 nickel (−1mL of an aqueous suspension) was added and the grey suspension was stirred vigorously. A balloon of hydrogen was attached to the flask via a three-way stopcock and hydrogen was allowed to slowly flow through the system for 1 minute. The flask was sealed under 1 atmosphere of hydrogen and vigorous stirring continued for 1 hour. The balloon was removed and the flask was flushed with argon. The suspension was gravity-filtered over fluted paper and washed with methanol. The filtrate was concentrated to a crude foam/glass and silica chromatography (70-90% ethyl acetate in n-hexanes with 1-3% methanol, followed by 1-6% methanol in dichloromethane) gave the title compound (0.35 g).

1. stirringvigorous stirring
2. waitcontinued for 1 hour
3. customThe balloon was removed
4. customthe flask was flushed with argon
5. filtrationThe suspension was gravity-filtered
6. washwashed with methanol
7. concentrationThe filtrate was concentrated to a crude foam/glass and silica chromatography (70-90% ethyl acetate in n-hexanes with 1-3% methanol, followed by 1-6% methanol in dichloromethane)