反应详情

温度

110 °C

A mixture of 4-methyl-2-((2S,3R)-3-methyl-2-(((5-(trifluoromethyl)pyridin-2-yl)amino)methyl)piperidine-1-carbonyl)benzonitrile (obtained from Example A22, 0.098 g, 0.235 mmol), TMSN3 (0.06 mL, 0.47 mmol) and SnO(n-Bu)2 (0.006 g, 0.024 mmol) in toluene (2 mL) was heated at 110° C. overnight. The mixture was cooled to rt and filtered through a pad of diatomaceous earth, washing with methanol. The solvent was removed in vacuo and the resulting crude residue was purified by reverse-phase preparative HPLC to obtain the title compound. ESI-MS (m/z): 460 [M+1]+.

1. temperatureThe mixture was cooled to rt
2. filtrationfiltered through a pad of diatomaceous earth
3. washwashing with methanol
4. customThe solvent was removed in vacuo
5. customthe resulting crude residue was purified by reverse-phase preparative HPLC