反应详情

2-{[3-(azidomethyl)-6-chloro-2-fluorophenyl]oxy}-6-chloro-4-pyridinecarbonitrile (0.402 g, 1.189 mmol) dissolved in THF (10 mL) was treated successively with triphenylphosphine (0.468 g, 1.783 mmol) and water (0.107 mL, 5.94 mmol) at 25° C. for 16 h with stirring. The reaction mixture was concentrated to dryness and purified on 40 g silica gel eluted successively with EtOAc (to remove tripheylphosphine oxide) followed by 0 to 10% CH3OH/DCM to give 2-{[3-(aminomethyl)-6-chloro-2-fluorophenyl]oxy}-6-chloro-4-pyridinecarbonitrile (0.161 g, 0.516 mmol, 43.4% yield) as a white solid. 1H NMR (400 MHz, DMSO-d6) δ ppm 7.96 (s, 1H), 7.93 (s, 1H), 7.44-7.55 (m, 2H), 3.77 (s, 2H), 1.94 (br. s., 2H). LC-MS (ES+) m/z 312.29, 314.28 [M+H].

1. concentrationThe reaction mixture was concentrated to dryness
2. custompurified on 40 g silica gel
3. washeluted successively with EtOAc (to remove tripheylphosphine oxide)