反应详情

温度

80 °C

An aqueous solution of NaOH 6N (70 mL, 420 mmol) was added to a solution of 4-(4-ethyl-5-fluoro-2-methoxyphenoxy)-3-fluorobenzonitrile (which may be prepared in accordance with the experimental described in Example 4, step 3; 4.0 g, 13.82 mmol) in methanol (140 mL). The reaction mixture was then stirred at reflux (80° C.) overnight. After cooling to 0° C., the reaction mixture was acidified by slow addition of concentrated HCl (25 mL) until pH=2. The mixture was then diluted by addition of ethyl acetate (300 mL) and the aqueous layer was separated and extracted with ethyl acetate (2×200 mL). The combined organic phases were dried over sodium sulfate, filtered and concentrated under vacuum to afford the title product as a beige solid (4.20 g, quantitative).

1. custommay be prepared in accordance with the
2. temperatureAfter cooling to 0° C.
3. customthe aqueous layer was separated
4. extractionextracted with ethyl acetate (2×200 mL)
5. dry with materialThe combined organic phases were dried over sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated under vacuum