反应详情

To a stirred solution of 3-(2,3-difluorophenyl)-1-ethylazetidin-3-ol (0.622 g, 2.91 mmol) in dichloromethane (30 mL) was added 3-chloroperoxybenzoic acid in portions (77%, 0.98 g, 4.37 mmol). The resulting mixture was stirred at ambient temperature for 5 h. The reaction mixture was poured onto a column of basic alumina, the column was washed with dichloromethane and eluated with methanol. Purification by HPLC on waters OBD C18, 5 μm (MeOH/33 mM NH3, 10:90 to 30:70) gave the title compound (0.160 g, 23.9%). The N-oxide was converted to the hydrochloric acid salt and recrystallized from methanol/acetonitrile. The product was analyzed by LCMS (Qtrap, Applied Biosystems, Q1 MS): MS (m+1)/z; 231 (M+1, bp).

1. additionThe reaction mixture was poured onto a column of basic alumina
2. washthe column was washed with dichloromethane
3. customPurification by HPLC on waters OBD C18, 5 μm (MeOH/33 mM NH3, 10:90 to 30:70)