反应详情

温度

70 °C

To a stirred solution of 3-{4-[5-(3,5-Dichloro-phenyl)-5-trifluoromethyl-4,5-dihydro-isoxazol-3-yl]-phenyl}azetidine-1-carboxylic acid tert-butyl ester (Preparation 40, 1 g, 1.94 mmol, 1 eq) in MeOH (10 mL) was purged HCl (g) at 0° C. for 0.5 hours and then reaction mixture was refluxed at 70° C. for 0.5 hours. Progress of reaction was monitored by TLC, after complete consumption of starting material reaction mixture was evaporated under reduced pressure to dryness to give 1.15 g (crude) Which was washed with methyl t-butyl ether (10 mL×2) to afforded 1.1 g (95.21%). 1H-NMR and LC-MS were consistent. 1H NMR (400 MHz, DMSO-d6) δ 4.05 (t, J=8 Hz, 2H), 4.15-4.21 (m, 1H), 4.24-4.39 (m, 4H), 7.55 (d, J=8 Hz, 2H), 7.62 (d, J=1 Hz, 2H), 7.74 (d, J=8 Hz, 2H), 7.81 (t, J=2 Hz, 1H), 8.99 (bs, 2H). LC-MS (m/z):=415 (M+H).

1. customreaction mixture
2. customProgress of reaction
3. customafter complete consumption of starting material reaction mixture
4. customwas evaporated under reduced pressure to dryness
5. customto give 1.15 g (crude) Which
6. washwas washed with methyl t-butyl ether (10 mL×2)
7. customto afforded 1.1 g (95.21%)