反应详情

温度

140 °C

A mixture of 4-(4-chloro-phenyl)-4-(4-iodo-phenyl)-piperidine and copper (I) cyanide in DMF was heated at 140° C. under nitrogen for 6 hours then allowed to cool. The mixture was diluted with ethyl acetate, washed with a mixture of conc. ammonia and brine (×5), dried (MgSO4), filtered and concentrated to give a residue which was partially purified by column chromatography (SiO2), eluting with a gradient of 2M ammonia in methanol (5% to 10%) and dichloromethane to afford the title compound (46 mg, <16%). This was taken on to the next reaction without further purification. LCMS (PS-A2) Rt 2.39 min [M+H]+ 297.

1. temperatureto cool
2. washwashed with a mixture of conc. ammonia and brine (×5)
3. dry with materialdried (MgSO4)
4. filtrationfiltered
5. concentrationconcentrated
6. customto give a residue which
7. customwas partially purified by column chromatography (SiO2)
8. washeluting with a gradient of 2M ammonia in methanol (5% to 10%) and dichloromethane