反应详情

tert-Butyl 3-(2-(4-(5-amino-6-cyano-4-(methylamino)pyridin-2-yl)-2-(trifluoro-methyl)phenoxy)ethyl)azetidine-1-carboxylate (100 mg) was dissolved in NMP (1000 μl) and hydrochloric acid (1M, 407 μl) added. A solution of sodium nitrite (20 mg) in water (150 μl) was added at room temperature and the reaction stirred for 1 hour. The reaction mixture was diluted with EtOAc (30 ml) and washed with water (3×20 ml) and brine (20 ml). Organics were dried over sodium sulphate and solvent evaporated under reduced pressure to yield crude product as a brown oil. Purification by flash chromatography (DCM to 2% MeOH in DCM mobile phase, 10 g silica column) afforded product tert-butyl 3-(2-(4-(4-cyano-1-methyl-1H-[1,2,3]triazolo[4,5-c]pyridin-6-yl)-2-(trifluoromethyl)phenoxy)ethyl)azetidine-1-carboxylate (84% yield).

1. washwashed with water (3×20 ml) and brine (20 ml)
2. dry with materialOrganics were dried over sodium sulphate and solvent
3. customevaporated under reduced pressure
4. customto yield crude product as a brown oil
5. customPurification by flash chromatography (DCM to 2% MeOH in DCM mobile phase, 10 g silica column)