Preparation method of alkyl-substituted diether type electron donor

A technology of electron donor and diether, which is applied in the field of preparation of diether electron donor, which can solve the problems of high synthesis cost and long reaction steps

Pending Publication Date: 2022-04-05
山东研峰新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process has the following limitations: 1. Due to the structure of the raw materials, it can only be used to synthesize 2-isoamyl-1,3-dimethoxypropane diether compounds; Hydrogen reaction, high synthesis cost; 3. Long reaction steps

Method used

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  • Preparation method of alkyl-substituted diether type electron donor
  • Preparation method of alkyl-substituted diether type electron donor
  • Preparation method of alkyl-substituted diether type electron donor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] The preparation technology of isopropyl-2-isoamyl-1,3-dimethoxypropane, the reaction equation is as follows:

[0039]

[0040] Wherein, R1 is isopropyl, R2 is isopentyl, and R3 is methyl.

[0041] The concrete reaction steps of above-mentioned reaction equation are as follows:

[0042] Step A, as shown in equation 1, under the protection of inert gas at room temperature, weigh 260g of sodium ethoxide-ethanol solution with a mass concentration of 17%, add it to a 3L reaction flask, and add 101g of compound a isopropylmalonic acid dropwise diethyl ester in the reaction flask, keep the temperature at 10-35°C, after the dropwise addition, stir for 2-4h; gradually add 90.5g of compound b bromoisopentane dropwise into the reaction flask, and monitor the reaction by gas chromatography Progress, when the mass concentration of diethyl isopropylmalonate of compound a is measured to be less than 5%, stop dripping compound b bromoisopentane to obtain reaction mixture 1; filter ...

Embodiment 2

[0049] The preparation process of isopropyl-2-isobutyl-1,3-dimethoxypropane, the reaction equation of this embodiment is the same as the reaction equation of embodiment 1:

[0050] The difference from Example 1 is that R1 is isopropyl, R2 is isobutyl, and R3 is methyl.

[0051] The specific preparation steps of isopropyl-2-isobutyl-1,3-dimethoxypropane in this embodiment are as follows:

[0052] Step A, under the protection of an inert gas at room temperature, weigh 1532g of potassium tert-butoxide-tetrahydrofuran solution with a mass concentration of 13.05%, add it to a 3L reaction flask, and add 296g of compound a diethyl isobutylmalonate dropwise to In the reaction flask, keep the temperature at 10-35°C. After the dropwise addition, stir for 2-4h; add 201g of compound b bromoisopropane dropwise into the reaction flask, and monitor the progress of the reaction by gas chromatography analysis, and measure the compound a isopropane When the mass concentration of butyldiethylma...

Embodiment 3

[0059] The preparation process of 4,4-bis(methoxymethyl)-2,6-dimethylheptane, the reaction equation of this embodiment is the same as the reaction equation of embodiment 1:

[0060] The difference from Example 1 is that R1 is isobutyl, R2 is isobutyl, and R3 is methyl.

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PUM

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Abstract

The invention relates to the technical field of diether type organic compounds, in particular to a preparation method of an alkyl-substituted diether type electron donor. The method comprises the following specific reaction steps: under the catalytic action of organic alkali, adding a compound b into a compound a, and carrying out an alkylation reaction of carbonyl alpha-carbon to obtain a compound c; carrying out ester reduction reaction on the compound c to obtain a compound d; and carrying out etherification reaction on the compound d and a compound e under the action of inorganic alkali to obtain a diether compound f. According to the invention, the alkyl diethyl malonate is adopted as a raw material and can be used for various alkyl-substituted diether electron donors, the intermediate treatment process is simple, other noble metal catalysts are not used, the product yield is high, the reaction route is short, and the preparation cost is low.

Description

technical field [0001] The invention relates to the technical field of diether organic compounds, in particular to a method for preparing an alkyl-substituted diether electron donor. Background technique [0002] The application of electron donors has played a very important role in the development of Ziegler-Natta catalysts for olefin polymerization. [0003] In 1990, Himont reported for the first time the introduction of diether electron donor compounds into the catalyst system. Compared with the fourth-generation diester catalysts, the prepared catalyst has obvious advantages, and is called the fifth-generation high-efficiency Ziegler-Natta catalyst. , there is not much literature on the synthesis of electron donors of such diethers. [0004] At present, the patent document CN201010296432.3 discloses a preparation method of a diether-type electron donor, using 1,3-methylbutyraldehyde as a raw material to obtain 2-isopropyl-5-methyl-2-hexyl through condensation reaction ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/16C07C29/147C07C67/343C07C43/10C07C31/20C07C69/34C07C69/50
Inventor 毕志强李晓强叶行培屈博扬王帆邓雄飞朱春磊
Owner 山东研峰新材料科技有限公司
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