反应详情

A suspension of 4-fluoro-2-methoxy-5-morpholin-4-yl-benzoic acid methyl ester (1.2.0 g, 4.46 mmol) in ethanol (22.0 mL) was treated with aq 2 N NaOH (13 mL, 26.7 mmol). The mixture was stirred at room temperature for 2 h, concentrated until most of the ethanol was removed and acidified with aq 2 N HCl to pH 1. After extracting with ethyl acetate, the organic layer was washed with saturated aq NaCl, dried over MgSO4 and concentrated to give 4-fluoro-2-methoxy-5-morpholin-4-yl-benzoic acid (0.90 g, 79%): 1H NMR (DMSO-d6 300 MHz) δ 12.62 (s, 1H), 7.34 (d, J=10.5 Hz, 1H), 7.04 (d, J=14.7 Hz, 1H), 3.76 (s, 3H), 3.70 (t, J=4.7 Hz, 4H), 2.90 (t, J=4.7 Hz, 4H).

1. concentrationconcentrated until most of the ethanol
2. customwas removed
3. extractionAfter extracting with ethyl acetate
4. washthe organic layer was washed with saturated aq NaCl
5. dry with materialdried over MgSO4
6. concentrationconcentrated