反应详情

A mixture of methyl 4-[({[5-chloro-2-(4-fluorophenoxy)pyridin-3-yl]carbonyl}amino)methyl]benzoate (step 1, 154 mg, 0.37 mmol), tetrahydrofuran (2 mL), methanol (2 mL), and 2 N sodium hydroxide (2 mL) was stirred at room temperature for 4 h. The mixture was poured into 1N hydrochloric acid (30 mL), and extracted with ethyl acetate (50 mL). The organic layer was dried over magnesium sulfate and evaporated. The residue was purified by TLC [dichloromethane/ethyl acetate (1:2)] to give 98 mg (66%) of the title compound as white solids: 1H-NMR (DMSO-d6) δ 9.13 (1H, t, J=6.0 Hz), 8.29 (1H, dd, J=2.6, 1.5 Hz), 8.22 (1H, dd, J=2.6, 1.5 Hz), 7.88 (2H, d, J=8.1 Hz), 7.47 (2H, d, J=8.1 Hz), 7.29–7.26 (4H, m), 4.60 (2H, d, J=6.0 Hz); MS (ESI) m/z 401 (M+H)+, 399 (M−H)−.

1. extractionextracted with ethyl acetate (50 mL)
2. dry with materialThe organic layer was dried over magnesium sulfate
3. customevaporated
4. customThe residue was purified by TLC [dichloromethane/ethyl acetate (1:2)]