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 MeOH, 50 mL THF and 50 mL 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 EtOAc (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 EtOAc (2×200 mL)
4. dry with materialthe combined extracts were dried over anhydrous sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated to dryness