反应详情

A mixture of 26.3 g. (0.0758 mole) of 4-(6-bromohexyl)-3,5-heptanedione, 13.1 g. (0.0787 mole) of ethyl p-hydroxybenzoate, 31.5 g. (0.228 mole) of powdered potassium carbonate, 4 g. of potassium iodide and 500 ml. of acetone was heated at reflux for 36 hours. The reaction mixture was concentrated in vacuo and partitioned between water and methylene dichloride. The organic layer was washed successively with sodium hydroxide solution, water, hydrochloric acid, water and sodium chloride solution, and then dried over anhydrous magnesium sulfate. The solution was concentrated and the residue crystallized and recrystallized from n-pentane to give 4-[10-(4-carbethoxyphenoxy)decyl]-3,5-heptanedione, m.p. 45°-46° C.

1. additionA mixture of 26.3 g
2. temperatureat reflux for 36 hours
3. concentrationThe reaction mixture was concentrated in vacuo
4. custompartitioned between water and methylene dichloride
5. washThe organic layer was washed successively with sodium hydroxide solution, water, hydrochloric acid, water and sodium chloride solution
6. dry with materialdried over anhydrous magnesium sulfate
7. concentrationThe solution was concentrated
8. customthe residue crystallized
9. customrecrystallized from n-pentane