反应详情

The 1-tert-butylpiperidine-4-carbonitrile (0.900 g, 5.41 mmol, (prepared as described in WO2008/1017461, Compound XXIV), ammonium sulfide (20 wt % in water, 3.69 mL, 10.8 mmol) and MeOH (9.0 mL) were heated in a CEM® microwave at about 120° C. for about 2 h (250 psi maximum pressure, 10 min ramp, 300 max watts). The mixture was concentrated under a stream of air and the resulting material was purified by flash chromatography on silica gel using DCM/MeOH with 3% NH4OH (8:2) as an eluent to give the title compound (0.140 g, 13%): LC/MS (Table 1, Method a) Rt=0.44 min; MS m/z: 201.1 (M+H)+.

1. concentrationThe mixture was concentrated under a stream of air
2. customthe resulting material was purified by flash chromatography on silica gel