تفاعل #5719

معادلة التفاعل

water

sodium methylate

dimethyl malonate

1-bromohexane

→

dimethyl n-hexylmalonate

المردود 78.3%

المذيبات

methanol

methanol

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONwere added dropwise
2. 2
   workup.STIRRINGAfter stirring at 40° for 1 hour
3. 3
   درجة الحرارةunder reflux for 2 hours, at 65°-69° for 2.5 hours
4. 4
   workup.ADDITIONwas added
5. 5
   workup.STIRRINGthe mixture was stirred
6. 6
   أخرىThe organic phase was separated
7. 7
   استخلاصThe aqueous phase was extracted with methylene chloride
8. 8
   أخرىthe combined organic extracts were dried
9. 9
   ترشيحfiltered
10. 10
    غسيلthe filter cake was washed with methylene chloride
11. 11
    تركيزthe combined filtrates were concentrated
12. 12
    workup.DISTILLATIONAfter distillation of the product there

الإجراء التجريبي

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.

المصدر