反应详情

温度

35 °C

5.75 g Sodium added in portions to 240 ml of methanol and the solution is heated to reflux for 1 hour. 28.4 ml Dimethylmalonate are added and the mixture is heated to reflux for another 10 minutes. The mixture is cooled to 35° C., 350 g 1-cyclobutylidenepropan-2-one (7% in 1,2-dichlorobenzene) are added and the mixture is refluxed for 1 hour. After recooling to room temperature a solution of 28.0 g potassium hydroxide in 130 ml water are added and the mixture is refluxed for 1 hour. The mixture is cooled to room temperature, the pH is adjusted to 1.5 by careful addition of half saturated hydrochloric acid and it is refluxed for 1 hour. The mixture is cooled to room temperature and the aqueous phase is extracted with ethyl acetate. The combined organic phases are dried over sodium sulfate, concentrated in vacuo and the residue is purified by chromatography on silica gel (petroleum ether/ethyl acetate 50:50).

1. temperaturethe solution is heated
2. temperatureto reflux for 1 hour
3. temperaturethe mixture is heated
4. temperatureto reflux for another 10 minutes
5. temperaturethe mixture is refluxed for 1 hour
6. customAfter recooling to room temperature
7. additionare added
8. temperaturethe mixture is refluxed for 1 hour
9. temperatureThe mixture is cooled to room temperature
10. temperatureis refluxed for 1 hour
11. temperatureThe mixture is cooled to room temperature
12. extractionthe aqueous phase is extracted with ethyl acetate
13. dry with materialThe combined organic phases are dried over sodium sulfate
14. concentrationconcentrated in vacuo
15. customthe residue is purified by chromatography on silica gel (petroleum ether/ethyl acetate 50:50)