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Synthetic method of preparing diisobutyl dimethyl malonate

A technology of diisobutyl dimethyl malonate and dimethyl malonate, applied in the field of synthesis of diisobutyl dimethyl malonate, can solve the problem of diisobutyl dimethyl malonate There are no literature reports on ester preparation methods, etc.

Inactive Publication Date: 2014-06-25
ZHANGJIAKOU SIRUIKAI TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But, the preparation method of diisobutyl dimethyl malonate has never been reported in the literature

Method used

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  • Synthetic method of preparing diisobutyl dimethyl malonate
  • Synthetic method of preparing diisobutyl dimethyl malonate
  • Synthetic method of preparing diisobutyl dimethyl malonate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] Example 1, 600 ml of anhydrous methanol was placed in a 1 L four-neck flask equipped with an electric stirrer, a thermometer, a 250 ml constant pressure dropping funnel and a condenser, and 89.1 g (1.65 mol) of sodium methoxide was added and heated to Reflux, quickly add 198 g (1.65 mol) dimethyl malonate dropwise, and react for 3-4 h after the addition, then slowly add 226 g (1.65 mol) bromoisobutane dropwise under slight reflux, dropwise for about 2 h After completion, keep reflux for another 16 h; then recover methanol under reduced pressure. After recovering methanol, add 600 ml of toluene, filter out insoluble matter, add 89.1 (1.65 mol) sodium methoxide, and depressurize to 0.085MPa to distill off the methanol generated by the reaction ; Then slowly drop 226 g (1.65 mol) of bromoisobutane, after about 1 h dropwise, keep reflux for 16 h, cool down to room temperature, slowly drop 20% dilute hydrochloric acid until the pH value reaches 4, separate the liquid , Disti...

Embodiment 2

[0011] Example 2, put 600 ml of anhydrous methanol into a 1 L four-neck flask equipped with electric stirring, a thermometer, a 250 ml constant pressure dropping funnel and a condenser, add 89.1 g (1.65 mol) of sodium methoxide, and heat to Reflux, quickly add 198 g (1.65 mol) dimethyl malonate dropwise, and react for 3-4 h after the addition, then slowly add 226 g (1.65 mol) chloroisobutane dropwise under slight reflux, dropwise for about 2 h After completion, keep reflux for another 16 h; then recover methanol under reduced pressure. After recovering methanol, add 600 ml of toluene, filter out insoluble matter, add 89.1 (1.65 mol) sodium methoxide, and depressurize to 0.085MPa to distill off the methanol generated by the reaction ; Then slowly drop 226 g (1.65 mol) of chloroisobutane, after about 1 h dropwise, keep reflux for 16 h, cool down to room temperature, slowly drop 20% dilute hydrochloric acid until the pH value reaches 4, separate the liquid , Distilled under reduc...

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Abstract

The invention discloses a synthetic method of preparing diisobutyl dimethyl malonate. The synthetic method is characterized in that dimethyl malonate and halogenated iso-butane are subjected to substitution reaction in different solvents in two steps so as to generate a target product. The synthetic method comprises the following steps: enabling sodium methylate to react with the dimethyl malonate, the halogenated iso-butane and methyl alcohol at a certain temperature so as to obtain an intermediate; and enabling the intermediate to react with the halogenated iso-butane and methylbenzene or xylene at a certain temperature, and after ending reaction, obtaining the high-purity diisobutyl dimethyl malonate through rectification, wherein the purity of the target product is greater than 99%.

Description

technical field [0001] The invention discloses a synthesis method for preparing dimethyl diisobutylmalonate. Background technique [0002] Hydrocarbyl malonate has been widely recognized in the industry as a metal ion chelating collector. CN102527523 reports a series of such compounds, and the application experiment results are good. Journal of Northeastern University (Natural Science Edition) 2007, vol.28, No.8, 1187-1189, reported malonate derivatives of benzyl groups and conducted applicability tests on the target compounds. Nonferrous Mining and Metallurgy 2012, vol.28, No.2, 18-20, reported malonic acid derivatives substituted by long-chain alkanes. In short, malonic acid and its derivatives have two carbonyl groups with strong chelating properties, which can have a strong coordination effect with metal ions. If the hydrocarbon group has a good hydrophobic effect, the application prospects of such compounds are very promising. broad. At the same time, hydrocarbyl mal...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/38C07C67/343
CPCC07C67/343C07C69/38
Inventor 不公告发明人
Owner ZHANGJIAKOU SIRUIKAI TECH
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