反应详情

A round bottom flask under nitrogen atmosphere was charged with cis-methyl 4-(3-nitropyridin-4-ylamino)cyclohexanecarboxylate (1.1 g, 3.94 mmol) and Pd/C (10% wt) (0.419 g, 0.394 mmol). EtOH (16 mL) was added, and the reaction mixture was purged with nitrogen 3 times. A H2-filled balloon was attached to the top of the flask, and the mixture stirred at RT for 2 hours. The reaction mixture was diluted with EtOH and filtered through Celite® brand filter aid. The pad was washed with DCM (50 mL), EtOH (50 mL), and MeOH (50 mL). The filtrate was concentrated to dryness to afford cis-methyl 4-(3-aminopyridin-4-ylamino)cyclohexanecarboxylate as a purple oil. (0.9 g, 92.0% yield). MS m/z=250.2 [M+H]. Calc'd for C13H19N3O2: 249.2.

1. customthe reaction mixture was purged with nitrogen 3 times
2. additionA H2-filled balloon
3. additionThe reaction mixture was diluted with EtOH
4. filtrationfiltered through Celite® brand
5. filtrationfilter aid
6. washThe pad was washed with DCM (50 mL), EtOH (50 mL), and MeOH (50 mL)
7. concentrationThe filtrate was concentrated to dryness