反应详情

温度

80 °C

A mixture of potassium carbonate (5.53 g, 0.04 mol) and 3-phenoxyphenol (15 g, 0.08 mol) in DMF (60 ml) was heated at 80° C. with stirring for 30 minutes. 2-Chloro-3-cyanopyridine (11.08 g, 0.08 mol) and copper bronze (0.8 g) were added and the resulting mixture heated at reflux for 90 minutes. GC analysis indicated the formation of a single product (96%). The reaction mixture was cooled and filtered, and then poured into water (300 ml) and allowed to stand over the weekend. The yellow-brown oily precipitate was extracted into dichloromethane and dried. The dichloromethane solution was then filtered and evaporated to yield crude 2-(3-phenoxyphenoxy)-3-cyano-pyridine (36.2 g, contaminated with DMF) which was used in the next stage without further purification.

1. temperaturethe resulting mixture heated
2. temperatureat reflux for 90 minutes
3. temperatureThe reaction mixture was cooled
4. filtrationfiltered
5. additionpoured into water (300 ml)
6. extractionThe yellow-brown oily precipitate was extracted into dichloromethane
7. customdried
8. filtrationThe dichloromethane solution was then filtered
9. customevaporated