反应详情

A mixture of 5-nitro-2-(4-(oxetan-3-yl)piperazin-1-yl)benzonitrile (9.8 g, 1.0 eq, 34.0 mmol) and Pd—C (10% loading, 3,6 g) in EtOH (300 mL) was stirred in a 500 mL round bottom flask. The reaction flask was evacuated under house vacuum and subsequently filled with hydrogen while stirring. This procedure was repeated three times and the reaction mixture was hydrogenated for 3 hours under an H2 balloon. The mixture was filtered through celite and the filter cake was washed with EtOH (2×50 mL). The filtrate was concentrated under vacuum to leave a white solid, which upon high vacuum drying gave 5-amino-2-(4-(oxetan-3-yl)piperazin-1-yl)benzonitrile in 93% yield.

1. customThe reaction flask was evacuated under house vacuum
2. additionsubsequently filled with hydrogen
3. stirringwhile stirring
4. filtrationThe mixture was filtered through celite
5. washthe filter cake was washed with EtOH (2×50 mL)
6. concentrationThe filtrate was concentrated under vacuum
7. customto leave a white solid, which upon high vacuum
8. customdrying