反应详情

温度

4 °C

To 98B (427 mg, 2.1 mmol) in anhydrous diethyl ether (10 mL) at 0° C. was added MeOH (0.87 mL, 10 eq.) and 4.0 N HCl in dioxane (4.2 mL, 16.8 mmol). The mixture was stirred at 4° C. for 24 h. Solvent was removed to give methyl 2-(2,4-difluoro-5-methoxyphenyl)-2-hydroxyacetimidate HCl salt. To this salt in CH2Cl2 (8.0 mL) was added H2O (8.0 mL). The mixture was stirred at rt for 30 min, then extracted with CH2Cl2 (2×50 mL). The combined organic extracts were dried and concentrated to give product 98C (493 mg, 99% yield) as a white solid. 1H NMR (400 MHz, CDCl3) δ ppm 3.41 (d, J=4.83 Hz, 1H) 3.72 (s, 3H) 3.80 (s, 3H) 5.32 (d, J=4.83 Hz, 1H) 6.78-6.84 (m, 1H) 6.90 (dd, J=9.01, 6.81 Hz, 1H).

1. customSolvent was removed