反应详情

温度

7.5 °C

To tert-butyl 4-(2-(4-(5-amino-6-cyano-4-(methylamino)pyridin-2-yl)-2-(trifluoromethyl)phenoxy)ethyl)piperidine-1-carboxylate (1.8 g) in NMP (20 ml) was added 1M hydrochloric acid (15 ml) and cooled to 5-10° C. with an ice bath. To above solution was then added dropwise a solution of sodium nitrite (0.335 g) in water (3 ml) during 2 minutes. The mixture was stirred further at room temperature for another 1 hour. After adding ethyl acetate (200 ml), the mixture washed with water (4×100 ml), brine (50 ml), solvent removed under reduced pressure and residue was columned on silica gel using 2:1 EtOAc:Heptane as eluant to give tert-butyl 4-(2-(4-(4-cyano-1-methyl-1H-[1,2,3]triazolo[4,5-c]pyridin-6-yl)-2-(trifluoromethyl)phenoxy)ethyl)-piperidine-1-carboxylate (1.55 g) as a white solid.

1. washthe mixture washed with water (4×100 ml), brine (50 ml), solvent
2. customremoved under reduced pressure and residue