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Method for preparing dimethyl n-butyl malonate

A technology of n-butyl dimethyl malonate and dimethyl malonate, which is applied in the field of n-butyl dimethyl malonate to prepare dimethyl n-butyl malonate, can solve the problem of high cost, Difficult product separation, complex preparation methods and other problems, to achieve the effect of low cost, simple operation, and easy to achieve reaction conditions

Inactive Publication Date: 2014-09-10
SHANGHAI INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] For the defects in the above-mentioned prior art, the technical problem to be solved by this invention is to provide a kind of method for preparing dimethyl n-butylmalonate, and this described method will solve the preparation method technology in the prior art Complexity, high cost, and difficult technical problems in product separation

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  • Method for preparing dimethyl n-butyl malonate
  • Method for preparing dimethyl n-butyl malonate

Examples

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Embodiment 1

[0021] 264.22g (227.78ml, 2.0mol) dimethyl malonate, 231.43g (260.03ml, 2.5mol) chlorobutane, 131.29g (0.95mol) anhydrous potassium carbonate powder, 438.55g (464.4ml, 6.0 mol) DMF, added to a three-necked flask, equipped with a condensing reflux device, a thermometer, heated and stirred, and the reaction temperature was 110-120°C. After reacting for 2 hours, in order to maintain the concentration of n-chlorobutane in the reaction, 185.14g (208.02 ml, 2.0mol) of n-chlorobutane was added to the reaction solution. The reflux reaction was continued for 3 hours, and 2.58 g (0.008 mol) of tetrabutylammonium bromide TBAB was added slowly, and the addition was completed in half an hour.

[0022] After adding the phase transfer catalyst, continue the reaction and track the reaction with GC, when the conversion rate of dimethyl malonate can reach 90% (GC analysis after about 6 hours). The reaction mixture was distilled off chlorobutane at 110-120°C, cooled, filtered, and the filtrate ...

Embodiment 2

[0025] 264.22g (227.78ml, 2.0mol) dimethyl malonate, 185.14g (208.02ml, 2.0mol) chlorobutane, 165.84g (1.20mol) anhydrous potassium carbonate powder, 511.64g (541.3ml, 7.0 mol) DMF, added to a three-necked flask, equipped with a condensing reflux device, a thermometer, heated and stirred, and the reaction temperature was 110-120°C. After reacting for 2 hours, in order to maintain the concentration of n-chlorobutane in the reaction, 231.43g (260.03ml, 2.5mol) of n-chlorobutane was added to the reaction solution. The reflux reaction was continued for 3 hours, and 2.58 g (0.008 mol) of tetrabutylammonium bromide TBAB was added slowly, and the addition was completed in half an hour.

[0026] After adding the phase transfer catalyst, continue the reaction and track the reaction with GC, when the conversion rate of dimethyl malonate can reach 90% (GC analysis after about 6 hours). The reaction mixture was distilled off chlorobutane at 110-120°C, cooled, filtered, and the filtrate w...

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Abstract

The invention relates to a method for preparing dimethyl n-butyl malonate, which comprises the following steps: weighing dimethyl malonate, an alkylation reagent, an inorganic alkali and a solvent, adding the dimethyl malonate and alkylation reagent into a reactor, adding the inorganic alkali and solvent, continuing stirring to react under heating reflux, supplementing chlorinated n-butane, adding a phase-transfer catalyst, continuing the reflux reaction, and collecting the product distilled at 110 DEG C under the pressure of 8 mmHg, thereby obtaining the dimethyl n-butyl malonate. The chlorinated n-butane is added in multiple steps to enhance the conversion rate of the dimethyl malonate; and after the chlorinated n-butane is recovered, fractionation is performed to obtain the product dimethyl n-butyl malonate. The method is economic and environment-friendly, has the advantages of low cost, no generation of disubstituted impurities and accessible reaction conditions, and is simple to operate and convenient for industrial production.

Description

technical field [0001] The invention belongs to the field of chemical engineering, and relates to a kind of dimethyl n-butylmalonate, in particular to a method for preparing dimethyl n-butylmalonate. Background technique [0002] Dimethyl n-butylmalonate (I), the English name is Dimethyl n-butylmalonate, [0003] [0004] (I) [0005] Colorless liquid with fruity aroma. Soluble in methanol, ethanol, ether and other organic solvents, insoluble in water. The relative density is 1.02, the boiling point is 219.6℃ / 760mmHg, and the refractive index is 1.425. Dimethyl n-butylmalonate is an important organic chemical raw material. Like its homologue diethyl n-butylmalonate, it is widely used in industries such as electrical chemicals, spices, medicine, and pesticides. In use, when used as a reaction intermediate, its superiority is far greater than that of diethyl n-butyl malonate, and the market prospect is extremely broad. [0006] At present, there are many documents on...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/46C07C67/343
CPCC07C67/343C07C69/46
Inventor 欧文华
Owner SHANGHAI INST OF TECH
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