反应详情

温度

25 °C

Five grams of 5-[3-hydroxy-4-(2-hydroxybenzoyl)-2-propylphenoxy]pentanenitrile, 11.7 g of potassium carbonate, and 1.42 ml of dimethyl sulfate in 50 ml of 2-butanone were stirred at reflux for approximately 18 hours. After cooling to 25° C., the mixture was partitioned between ethyl acetate and water. The organic layer was separated, washed with one volume of water and one volume of a saturated sodium chloride solution, dried over magnesium sulfate, filtered, and evaporated to dryness leaving a yellow oil which crystallized on standing. Recrystallization from ethyl acetate/hexane provided 4.38 g of the desired title product, m.p. 85°-86.5° C.

1. temperatureat reflux for approximately 18 hours
2. customthe mixture was partitioned between ethyl acetate and water
3. customThe organic layer was separated
4. washwashed with one volume of water and one volume of a saturated sodium chloride solution
5. dry with materialdried over magnesium sulfate
6. filtrationfiltered
7. customevaporated to dryness
8. customleaving a yellow oil which
9. customcrystallized
10. customRecrystallization from ethyl acetate/hexane