反应详情

A mixture of {trans-4-[(6-nitrothieno[3,2-b]pyridin-7-yl)amino]cyclohexyl}methanol (0.080 g, 0.26 mmol) (Example 2, Step 1) and 10% palladium on carbon (0.03 g) in methanol (3 mL) was hydrogenated under balloon pressure of H2 at room temperature for 1 h. The mixture was filtered. The filtrate was concentrated, diluted with dichloromethane, then dried over MgSO4, and concentrated. The residue was purified on silica gel (eluting with 10% MeOH in dichloromethane) to give the desired product (41 mg, 57%). LCMS calculated for C14H20N3OS (M+H)+: m/z=278.1. Found: 278.1.

1. filtrationThe mixture was filtered
2. concentrationThe filtrate was concentrated
3. additiondiluted with dichloromethane
4. dry with materialdried over MgSO4
5. concentrationconcentrated
6. customThe residue was purified on silica gel (eluting with 10% MeOH in dichloromethane)