反应详情

Under nitrogen atmosphere free of water and oxygen, to a three-necked flask equipped with a dropping funnel were successively added 0.15 mol of potassium tert-butoxide and 150 ml of THF, then stirrer was started. 0.12 Mol of methyl acetoacetate was slowly dropped to the reactor cooled in an ice-water bath. Upon completion of the dropping, the reaction was continued at room temperature for further 1 hr. Then 0.18 mol of ethyl iodide was slowly dropped at room temperature, and then the reaction was heated to reflux for 6 hrs. At the end of the reaction, solvent was evaporated by using a rotatory evaporator, and saturated saline was added to just dissolve the solid. Organic phase was separated, and aqueous phase was extracted with a suitable amount of diethyl ether for three times. The combined organic phase was washed well with saturated saline, then dried over anhydrous sodium sulfate. Solvent was removed by using a rotatory evaporator, and the residue was distilled under reduced pressure to give 0.072 mol of product. Yield 60%.

1. customstirrer was started
2. temperaturecooled in an ice-water bath
3. temperaturethe reaction was heated
4. temperatureto reflux for 6 hrs
5. customAt the end of the reaction, solvent
6. customwas evaporated
7. customa rotatory evaporator, and saturated saline
8. additionwas added
9. dissolutionto just dissolve the solid
10. customOrganic phase was separated
11. extractionaqueous phase was extracted with a suitable amount of diethyl ether for three times
12. washThe combined organic phase was washed well with saturated saline
13. dry with materialdried over anhydrous sodium sulfate
14. customSolvent was removed
15. customa rotatory evaporator
16. distillationthe residue was distilled under reduced pressure