反应详情

温度

50 °C

To a solution of methyl 2-methyl-2-(4-trifluoromethyl-2-pyridyloxy)propionate (Step B, 7.5 g, 29 mol) in 50 mL of methanol, 50 mL of tetrahydrofuran and 50 mL of water was added sodium hydroxide (2.3 g, 57 mmol). After stirring at 50° C. for 5 h, the reaction mixture was partially concentrated, and was added 2 M hydrochloric acid to pH>2. The resulting mixture was extracted with ethyl acetate (2×200 mL), and the combined extracts were dried over anhydrous sodium sulfate, filtered, and concentrated to dryness to afford the title compound. 1H NMR (500 MHz, CD3OD): δ 8.28 (d, 1H), 7.17 (d, 1H), 7.05 (s, 1H), 1.70 (s, 6H).

1. concentrationthe reaction mixture was partially concentrated
2. additionwas added 2 M hydrochloric acid to pH>2
3. extractionThe resulting mixture was extracted with ethyl acetate (2×200 mL)
4. dry with materialthe combined extracts were dried over anhydrous sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated to dryness