反应详情

To a stirred mixture of trans-4-{2-[4-(2,3-dihydrofuro[3,2-c]pyridin-4-yl)-piperazin-1-yl]-ethyl}-cyclohexanamine trihydrochloride (intermediate C) (110 mg, 0.25 mmol) in DMF (1.8 ml) was added N,N-diisopropylethylamine (210 mg, 278 μl, 1.63 mmol), acetic acid (18.0 mg, 17.2 μl, 300 μmol) and TBTU (128 mg, 400 μmol). The mixture was allowed to stir at room temperature for 4 h. The mixture was added to 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 (0.15 g) was triturated with dichloromethane (2 ml) and diethyl ether (5 ml) for ½ h, the precipitate was collected by filtration, washed with diethyl ether and dried to yield the title compound as off-white solid (92 mg, 99%), MS (ISP) m/z=373.2 [(M+H)+], mp 260° 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 (0.15 g) was triturated with dichloromethane (2 ml) and diethyl ether (5 ml) for ½ h
6. filtrationthe precipitate was collected by filtration
7. washwashed with diethyl ether
8. customdried