反应详情

温度

0 °C

In a 2 L flask, 2-(4-amino-3-methylphenoxy)-5-fluorobenzonitrile (277.1 ml, 221.7 mmol) was taken up in toluene (0.8 M) and treated with potassium acetate (26.11 g, 266.0 mmol) at ambient temperature. The reaction mixture was cooled to 0° C. and acetic anhydride (63.91 mL, 676.1 mmol) was added over 2 minutes. The ice bath was removed, the flask was fitted with a reflux condenser and the reaction was heated to 40° C. Isoamyl nitrite (59.29 mL, 443.3 mmol) was added dropwise. The reaction was heated to reflux for 15 hours, cooled to ambient temperature, and concentrated. The resulting solids were suspended in 2 L water, stirred vigorously for 15 minutes, filtered, and washed with water (1 L). The resulting solid (75 g, still wet) was used directly in the next step.

1. customThe ice bath was removed
2. customthe flask was fitted with a reflux condenser
3. temperaturethe reaction was heated to 40° C
4. temperatureThe reaction was heated
5. temperatureto reflux for 15 hours
6. temperaturecooled to ambient temperature
7. concentrationconcentrated
8. filtrationfiltered
9. washwashed with water (1 L)