Diethyl butylmalonate synthesis
- Product Name:Diethyl butylmalonate
- CAS Number:133-08-4
- Molecular formula:C11H20O4
- Molecular Weight:216.27
Yield:133-08-4 92%
Reaction Conditions:
Stage #1:diethyl malonate with copper(l) chloride for 1.5 h;Large scale;
Stage #2:N-butylamine for 10 h;Reflux;Large scale;Time;
Steps:
1
In the installation of a stirrer,thermometer,Reflux condenser,In the reaction vessel of the dropping funnel,Adding dichloroethylamine 3L,62 mol of cuprous chloride was added in portions to control the stirring speed of 150 rpm,Raise the temperature of the solution to 75 ° C,Reaction time 4h,A solution of diethyl malonate (2)Plus continue to stir after 90min,The addition of n-butylamine (3)6.8 mol,Reaction time 6h,Then reflux 4h,The dichloroethylamine was distilled off under reduced pressure,Reduce the temperature of the solution to 18 , add 3L mass fraction of 20% sodium chloride solution, keep the stirring speed 190rpm for 70min, separate the water layer, the oil layer 2.3kP vacuum distillation,A fraction of 130-135 ° C was collected,Potassium sulfate solution, the mass fraction of 80% hexane, in the mass fraction of 98% ethyl acetate in the recrystallization,1212.19 g of diethyl n-butylmalonate was obtained in a yield of 92%.
References:
Chengdu kadifu Technology Co. Ltd;Liao, ruer CN105461558, 2016, A Location in patent:Paragraph 0007; 0015; 0016
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