反应详情

To a solution of 2-{1-[2-(2,4-difluorophenyl)ethyl]azetidin-3-yl}-1-phenylethanone (Example 20, 41 mg, 0.117 mmol) in methanol (1 mL) under nitrogen was added sodium borohydride (8.8 mg, 0.23 mmol). The reaction was stirred at room temperature overnight. More sodium borohydride (5 mg, 0.13 mmol) was added and the reaction stirred for 30 minutes. More sodium borohydride (8.8 mg, 0.23 mmol) was added and the reaction stirred for 15 minutes. More sodium borohydride (5 mg, 0.13 mmol) was added and the reaction stirred overnight. The solvent was removed in vacuo and the residue purified by flash column chromatography on silica, eluting with 10% methanol/dichloromethane, to give the title compound. 1H NMR (360 MHz, CDCl3) δ 7.35–7.29 (5H, m), 7.22–7.16 (1H, m), 6.81–6.73 (2H, m), 4.71 (1H, dd, J=5.3, 7.6 Hz), 3.63 (1H, s), 3.53 (1H, s), 3.11 (1H, s), 2.98 (1H, s), 2.77 (5H, s), 2.07–1.92 (2H, m); m/z (ES+) 318 (M+H)+.

1. stirringthe reaction stirred for 30 minutes
2. stirringthe reaction stirred for 15 minutes
3. stirringthe reaction stirred overnight
4. customThe solvent was removed in vacuo
5. customthe residue purified by flash column chromatography on silica
6. washeluting with 10% methanol/dichloromethane