反应详情

Diethylmalonate (80.0g) in ethyl alcohol (50ml) was added to a solution of sodium ethoxide (prepared from sodium metal (13.0g) and absolute alcohol (400ml)) over 15 minutes whilst gently refluxing the mixture. After stirring under reflux for 1 hour a solution of 2-bromopropane (74.5g) in alcohol (50ml) was added over 1 hour and the mixture stirred under reflux overnight. The reaction mixture was cooled in ice and inorganic material removed by filtration and the filtrate concentrated. Water was added to the concentrate which was extracted with ether, the ethereal extracts washed with 2N sodium hydroxide solution (X2) and dried over magnesium sulphate. Removal of solvent gave an almost colourless liquid which was further purified by distillation to give diethyl isopropylmalonate b.p. 62°-65° C/0.7 mm Hg.

1. temperaturegently refluxing the mixture
2. additionwas added over 1 hour
3. stirringthe mixture stirred
4. temperatureunder reflux overnight
5. temperatureThe reaction mixture was cooled in ice
6. custominorganic material removed by filtration
7. concentrationthe filtrate concentrated
8. additionWater was added to the
9. concentrationconcentrate which
10. extractionwas extracted with ether
11. washthe ethereal extracts washed with 2N sodium hydroxide solution (X2)
12. dry with materialdried over magnesium sulphate
13. customRemoval of solvent
14. customgave an almost colourless liquid which
15. distillationwas further purified by distillation