反应详情

A solution of 1.3 g of sodium metal in 30 ml of ethanol is treated with 9 g of diethylmalonate and an ethanolic solution of 12.1 g of 3,4-dichlorobenzalacetone, heated under reflux for 15 min, cooled and concentrated to dryness in vacuo. The residue is treated with 400 ml of water containing 7 g of 80% potassium hydroxide pellets and heated under reflux for 2 hr. Insoluble material is removed and the filtrate is acidified with concentrated sulfuric acid, heated under reflux until carbon dioxide evolution ceases, cooled, filtered, washed with water and dried. Recrystallization from 2-propanol gives 5-(3,4-dichlorophenyl)-1,3-cyclohexanedione; mp 198°-200° C.

1. temperatureunder reflux for 15 min
2. temperaturecooled
3. concentrationconcentrated to dryness in vacuo
4. additionThe residue is treated with 400 ml of water containing 7 g of 80% potassium hydroxide pellets
5. temperatureheated
6. temperatureunder reflux for 2 hr
7. customInsoluble material is removed
8. temperatureheated
9. temperatureunder reflux until carbon dioxide evolution ceases
10. temperaturecooled
11. filtrationfiltered
12. washwashed with water
13. customdried
14. customRecrystallization from 2-propanol