反应详情

350.1 g of 30 percent sodium methylate solution in methanol were diluted with 550 ml of methanol under nitrogen and while stirring. 264.2 g of dimethyl malonate were added dropwise. After warming the suspension to 40° 321.0 g of 1-bromohexane were added dropwise. After stirring at 40° for 1 hour, under reflux for 2 hours, at 65°-69° for 2.5 hours and cooling the suspension to room temperature water was added and the mixture was stirred. The organic phase was separated. The aqueous phase was extracted with methylene chloride, the combined organic extracts were dried and filtered, the filter cake was washed with methylene chloride and the combined filtrates were concentrated. After distillation of the product there were obtained 329.3 g (78.3%) of dimethyl n-hexylmalonate.

1. additionwere added dropwise
2. stirringAfter stirring at 40° for 1 hour
3. temperatureunder reflux for 2 hours, at 65°-69° for 2.5 hours
4. additionwas added
5. stirringthe mixture was stirred
6. customThe organic phase was separated
7. extractionThe aqueous phase was extracted with methylene chloride
8. customthe combined organic extracts were dried
9. filtrationfiltered
10. washthe filter cake was washed with methylene chloride
11. concentrationthe combined filtrates were concentrated
12. distillationAfter distillation of the product there