反应详情

Under nitrogen atmosphere, to a reactor was added 0.22 mol of potassium tert-butoxide. After evacuating for 2 hrs, 80 ml of THF was added to dissolve the solid with stirring. Then 0.1 mol of butyl acetoacetate was slowly dropped to the reactor cooled in an ice-water bath, and the reaction was continued for further 2 hrs. Then under cooled in the ice-water bath, 0.12 mol of isobutyryl chloride was slowly dropped, and the reaction was continued for further 1.5 hrs. Next, under cooled in the ice-water bath, water was added to dissolve resultant solid, and the reaction mixture was neutralized with hydrochloric acid. Diethyl ether was used to extract product, and the collected organic layer was dried over anhydrous sodium sulfate. Removing solvent by using a rotatory evaporator gave the product.

1. customAfter evacuating for 2 hrs
2. addition80 ml of THF was added
3. dissolutionto dissolve the solid
4. temperaturecooled in an ice-water bath
5. additionwas slowly dropped
6. waitthe reaction was continued for further 1.5 hrs
7. additionwas added
8. dissolutionto dissolve resultant solid
9. extractionto extract product
10. dry with materialthe collected organic layer was dried over anhydrous sodium sulfate
11. customa rotatory evaporator
12. customgave the product