反应详情

To the solution of 2-(2-azido-1,1-difluoro-ethyl)-pyridine N-oxide (example 60a, 2.7 g, 13.5 mmol) in THF (40 mL) was slowly added triphenylphosphine (3.9 g, 14.9 mmol) at 0° C. After stirred for 1 h, water (5 mL) was added. The reaction mixture was stirred at 55° C. for 2 h and at room temperature for 12 h. After removal of solvent, the crude was puried by flash chromatography (Merck Silica gel 60, 70-230 mesh, 0%-20% methanol in methylene chloride in 30 min) to give 2,2-difluoro-2-pyridin-2-yl-ethylamine N-oxide (2.2 g, 96%) as a white solid. LC-MS m/e 175 (MH+).

1. customat 0° C
2. stirringThe reaction mixture was stirred at 55° C. for 2 h and at room temperature for 12 h
3. customAfter removal of solvent
4. customwas puried by flash chromatography (Merck Silica gel 60, 70-230 mesh, 0%-20% methanol in methylene chloride in 30 min)