Method for preparing 2,3-dialkyl succinic acid and ester compounds thereof

A technology of dihydrocarbyl succinic acid and compounds, which is applied in two fields, and can solve problems such as not being disclosed, not being suitable for industrialization, etc.

Active Publication Date: 2009-04-01
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, it is not suitable for industrialization
Although the CN1313869A document discloses 2,3-dicyclohexyl diethyl succinate embodiment and it can be prepared by the esterification and reduction reaction of 2,3-diphenylsuccinic acid, there is no disclosure of 2,3-diethyl succinate The specific preparation method of phenylsuccinic acid

Method used

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  • Method for preparing 2,3-dialkyl succinic acid and ester compounds thereof
  • Method for preparing 2,3-dialkyl succinic acid and ester compounds thereof
  • Method for preparing 2,3-dialkyl succinic acid and ester compounds thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1～5

[0146] Examples 1-5, preparation of 1,2-dihydrocarbyl-1,1,2,2-tetrakis(alkoxycarbonyl)ethane.

Embodiment 1

[0147] Example 1: Preparation of 1,2-diphenyl-1,1,2,2-tetrakis(ethoxycarbonyl)ethane

[0148] Add 3.0 g of sodium hydride into a 250 ml one-necked flask. Then add 25ml of petroleum ether and shake to dissolve the mineral oil protecting sodium hydride in petroleum ether. Let it stand again to make the sodium hydride settle down. Pour out the petroleum ether, and then add 25ml petroleum ether into the one-mouth bottle. Wash like this three times. Then the residual petroleum ether was removed with a rotary evaporator. Remove the single-necked bottle, weigh 1.7 g of sodium hydride by differential gravimetric method, and quickly add 50 ml of dried tetrahydrofuran.

[0149] Weigh 11.8 g of diethyl phenylmalonate, and slowly add it dropwise into a single-necked bottle filled with sodium hydride. As the dropwise addition proceeded, bubbles emerged from the reaction solution. After the dropwise addition was completed, the reaction was continued for 1 hour to obtain a reaction sol...

Embodiment 2

[0155] Example 2: Preparation of 1,2-diphenyl-1,1,2,2-tetrakis(ethoxycarbonyl)ethane

[0156] Weigh 0.39 g of potassium metal by differential gravimetric method, and add it into 10 ml of absolute ethanol three times to obtain an ethanol solution of potassium ethoxide.

[0157] Add 2.36 g of diethyl phenylmalonate in a 100 ml one-necked flask, and then add 15 ml of absolute ethanol. Then, under the condition of stirring, the ethanol solution of potassium ethoxide was added dropwise into diethyl phenylmalonate with a constant pressure dropping funnel, and the reaction was carried out for 1 hour. Ethanol was then removed under reduced pressure to give a white solid. 15ml of dimethyl sulfoxide (DMSO) was added thereto, and the white solid was completely dissolved to obtain a reaction solution.

[0158] Weigh 1.27g of elemental iodine and dissolve it in 10ml of dimethyl sulfoxide (DMSO) to prepare an iodine solution. Then, at room temperature (about 20° C.), a DMSO solution of i...

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Abstract

The invention relates to a preparation method of 2, 3-dialkyl succinic acid and ester compounds thereof. 1, 2-dialkyl-1, 1, 2, 2-tetra (alkoxy carbonyl)ethane is prepared through the dimerization coupling reaction of 2-alkyl-malonic ester compounds, then the 2, 3-dialkyl succinic acid is prepared by carrying out hydrolysis and decarboxylation reaction, and the 2, 3-dialkyl succinate compounds are prepared by further esterification. The preparation method is conductive to the commercial production of the 2, 3-dialkyl succinate and can be used for preparing a Ziegler-Natta polypropylene catalyst as an internal electron donor compound. The preparation method can be used in the technical field of petrochemical polypropylene.

Description

technical field [0001] The invention relates to a preparation method of organic compounds, in particular to a preparation method of 2,3-dihydrocarbyl succinic acid and ester compounds thereof. Background technique [0002] Searching for ideal electron donor compounds has always been a hot spot in the research of new polypropylene catalysts. The existing document CN1313869A discloses that succinate compounds are used as one of the catalyst components for the preparation of solid catalysts for olefin polymerization. Among them, the succinate of formula (IV) is a particularly preferred internal electron donor compound. The series of succinates are internal electron donors of Ziegler-Natta catalysts, which improve the ability of catalysts to control the relative molecular mass distribution, isotacticity and oligomer content of olefin polymers. Using this catalyst can not only improve the impact strength of the product, but also maintain the flexural modulus; or increase the fl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C55/02C07C51/38
Inventor 谢伦嘉李志强田宇赵思源亢宇冯华升
Owner CHINA PETROLEUM & CHEM CORP
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