反应详情

A solution of 2-(5,5-dimethyl-3-(3-nitropyridin-4-yl)cyclohex-2-enyl)isoindoline-1,3-dione (1 eq) in Acetic Acid (0.1 M) was purged with nitrogen for 10 min. Then 10% Pd/C (0.10 eq) was added. The reaction mixture was stirred at room temperature overnight an atmosphere of hydrogen. Solids were removed by filtration over celite, then rinsed with EtOAc and MeOH. The filtrate was concentrated, diluted with EtOAc and washed 2× with sat. aq. 2M Na2CO3. Organic layer was dried with MgSO4, filtered, and concentrated. The residue was purified by column (5% methanol in 1:1 ethyl acetate and hexanes) to give 2-(3-(3-aminopyridin-4-yl)-5,5-dimethylcyclohex-2-enyl)isoindoline-1,3-dione (89%). LC/MS (m/z): MH+=348.3, Rt=0.79 min.

1. customSolids were removed by filtration over celite
2. washrinsed with EtOAc and MeOH
3. concentrationThe filtrate was concentrated
4. additiondiluted with EtOAc
5. washwashed 2× with sat. aq. 2M Na2CO3
6. dry with materialOrganic layer was dried with MgSO4
7. filtrationfiltered
8. concentrationconcentrated
9. customThe residue was purified by column (5% methanol in 1:1 ethyl acetate and hexanes)