反应详情

To a stirred solution of 3-{4-[5-(3,5-dichloro-phenyl)-5-trifluoromethyl-4,5-dihydro-furan-3-yl]-phenyl}-3-fluoro-azetidine-1-carboxylic acid tert-butyl ester (Example 1, Intermediate 2) (0.45 g, 0.845 mmol) in MeOH (10 mL) was purged HCl gas for 1 hour at room temperature. After consumption of starting material, reaction mixture concentrated in vacuo to get pale yellow semisolid (0.49 g, crude), which was triturated with n-pentane (2×5 mL) to get off product as white solid. Yield: 0.36 g, 98.53%. 1H NMR (400 MHz, DMSO-d6) δ: 3.20 (d, J=17.16 Hz, 1H), 3.64 (d, J=17.16 Hz, 1H), 4.30-4.54 (m, 4H), 7.29 (d, J=7.96 Hz, 2H), 7.48 (s, 1H), 7.52 (d, J=8 Hz, 2H), 7.69-7.71 (m, 3H), 9.36 (bs, 2H).

1. customAfter consumption of starting material, reaction mixture
2. concentrationconcentrated in vacuo
3. customto get pale yellow semisolid (0.49 g, crude), which
4. customwas triturated with n-pentane (2×5 mL)
5. customto get off product as white solid