反应详情

A solution of (4-hydroxyphenyl)propan-2-one ethylene ketal (28 g) in ethanol (40 ml) was added to a stirred solution of sodium ethoxide in ethanol (7.1 g of sodium in 100 ml) and the resulting solution stirred at room temperature for 20 minutes. A suspension of 2-picolyl chloride hydrochloride (25 g) in ethanol (60 ml) was added and the resulting mixture was boiled under reflux for 5 hours, cooled and filtered. 2M Hydrochloric acid (100 ml) was added, the solution boiled for 5 h, cooled and neutralised with 2M sodium hydroxide solution. After dilution with water the solution was extracted with dichloromethane and the washed organic phase dried and evaporated to give a dark oil. Bulb to bulb distillation gave [4-(2-pyridylmethyloxy)phenyl]propan-2-one, b.pt. 96°-100° C./0.2 mm, which was used without further purification.

1. additionwas added
2. temperatureunder reflux for 5 hours
3. temperaturecooled
4. filtrationfiltered
5. addition2M Hydrochloric acid (100 ml) was added
6. waitthe solution boiled for 5 h
7. temperaturecooled and neutralised with 2M sodium hydroxide solution
8. extractionAfter dilution with water the solution was extracted with dichloromethane
9. customthe washed organic phase dried
10. customevaporated
11. customto give a dark oil
12. distillationBulb to bulb distillation