反应详情

To a stirred mixture of trans-4-{2-[4-(2,3-dihydro-furo[2,3-c]pyridin-7-yl)-piperazin-1-yl]-ethyl}-cyclohexylamine trihydrochloride (intermediate B) (132 mg, 0.3 mmol) in DMF (2.2 ml) was added N,N-diisopropylethylamine (252 mg, 334 μl, 1.95 mmol), acetic acid (21.6 mg, 20.6 μl, 360 μmol) and TBTU (154 mg, 480 μmol). The mixture was allowed to stir at room temperature for 4 h, poured into ice/water (5 ml) and 1N NaOH (5 ml) and extracted with dichloromethane/MeOH (9:1, 20 ml). The organic phase was washed with brine (20 ml), dried (MgSO4) and evaporated. The crude material (0.13 g) was triturated with dichloromethane (1 ml) and heptane (5 ml) for 30 min, the precipitate was collected by filtration, washed with heptane and dried to yield the title compound as a white solid (95 mg, 85%), MS (ISP) m/z=372.9 [(M+H)+], mp 195° C.

1. extractionextracted with dichloromethane/MeOH (9:1, 20 ml)
2. washThe organic phase was washed with brine (20 ml)
3. dry with materialdried (MgSO4)
4. customevaporated
5. customThe crude material (0.13 g) was triturated with dichloromethane (1 ml) and heptane (5 ml) for 30 min
6. filtrationthe precipitate was collected by filtration
7. washwashed with heptane
8. customdried