反应详情

To a solution of 2-(3-(3-nitropyridin-4-yl)cyclohex-2-enyl)isoindoline-1,3-dione (1.0 equiv.) in acetic acid (0.1 M) was added 10% Pd/C (0.2 equiv.) and the reaction was stirred under a H2 balloon. After 3 days, the reaction was filtered through Celite, washed with ethyl acetate and methanol, the filtrate was diluted with ethyl acetate and washed twice with sat. 2M Na2CO3. The organic phase was dried with magnesium sulfate, filtered and concentrated. The crude material was triturated with hexanes and ethyl acetate to afford 2-(3-(3-aminopyridin-4-yl)cyclohexyl)isoindoline-1,3-dione in 73% yield. LC/MS=322.2 (M+H), Rt=0.64 min.

1. filtrationthe reaction was filtered through Celite
2. washwashed with ethyl acetate and methanol
3. additionthe filtrate was diluted with ethyl acetate
4. washwashed twice with sat. 2M Na2CO3
5. dry with materialThe organic phase was dried with magnesium sulfate
6. filtrationfiltered
7. concentrationconcentrated
8. customThe crude material was triturated with hexanes and ethyl acetate