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A preparation method of organosilicon compound containing anthracene-protected α-cyanoacryloyloxy structure

A technology for cyanoacryloyloxy and organosilicon compounds, which is applied in the field of preparation of organosilicon compounds, can solve the problems of harsh reaction conditions, many by-products, and little environmental pollution, and achieves a single product composition, mild reaction conditions, and ease of use. The effect of separation and purification

Active Publication Date: 2020-06-19
HANGZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] In order to solve the problems of harsh reaction conditions, many by-products and low yield of the target product in the existing preparation of organosilicon polymers containing anthracene-protected α-cyanoacryloyloxy structures, the present invention proposes an anthracene-protected The preparation method of organosilicon compounds with α-cyanoacryloyloxy structure has the characteristics of low energy consumption, little environmental pollution, safety and environmental protection, high yield, easy separation of products, simple process and equipment, and low production cost.

Method used

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  • A preparation method of organosilicon compound containing anthracene-protected α-cyanoacryloyloxy structure
  • A preparation method of organosilicon compound containing anthracene-protected α-cyanoacryloyloxy structure
  • A preparation method of organosilicon compound containing anthracene-protected α-cyanoacryloyloxy structure

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Add 20mL of DMF solvent to a 100mL three-necked flask equipped with a condenser, a thermometer and electromagnetic stirring, and add 3.13g (0.01mol) anthracene-protected α-cyanoacrylate potassium salt, 2.48g (0.0103mol) γ-chloro Propyltriethoxysilane, 0.311g halogenation reaction catalyst potassium iodide, 0.0319g esterification reaction catalyst 4-dimethylaminopyridine, then heat up to 120°C, react at this temperature for 2h and then cool down to room temperature, and filter the crude reaction product After removing the by-product KCl, slowly add the collected filtrate dropwise at a rate of 1-2 drops per second to 100mL of 12% sodium chloride aqueous solution under stirring, and let stand for 2h after the dropwise addition, and wait for the product After settling, separate the liquid to remove the upper water layer, add 40mL of dichloromethane lysates to the collected organic layer, then add 80mL of deionized water in the dichloromethane solution, wash off the residual ...

Embodiment 2

[0044] Add 50mL of DMAC (N,N-dimethylacetamide) solvent to a 250mL three-necked flask equipped with a condenser, a thermometer and electromagnetic stirring, and add 3.13g (0.01mol) of anthracene-protected potassium α-cyanoacrylate under stirring at room temperature Salt, 11.91g (0.0495mol) γ-chloropropyl triethoxysilane, 0.783g halogenation reaction catalyst potassium bromide, 0.1565g esterification reaction catalyst 2-dimethylaminopyridine, then be heated to 120 ℃, at this Cool down to room temperature after reacting for 5 hours at high temperature. After filtering the crude reaction product to remove the by-product KCl, slowly add the collected filtrate dropwise to 180 mL of sodium chloride with a mass fraction of 13% under stirring at a rate of 1-2 drops per second. In the aqueous solution, let it stand for 2 hours after the dropwise addition. After the product settles, separate the liquid to remove the upper water layer, add 110 mL of dichloromethane dissolved product to th...

Embodiment 3

[0046] Add 20mL DMSO (dimethyl sulfoxide) solvent to a 100mL three-necked flask equipped with a condenser tube, a thermometer and electromagnetic stirring, and add 3.13g (0.01mol) anthracene-protected α-cyanoacrylate potassium salt under stirring at room temperature, 2.98g ( 0.015mol) γ-chloropropyltrimethoxysilane, 0.157g halogenation reaction catalyst sodium iodide, 0.017g esterification reaction catalyst 4-aminopyridine, then heat up to 100°C, react at this temperature for 5h and then cool down to room temperature After the reaction crude product was filtered to remove the by-product KCl, the collected filtrate was slowly added dropwise at a rate of 1-2 drops per second to 70mL of 9% sodium chloride aqueous solution with a mass fraction of 9% under stirring. Set aside for 6h, after the product settles, remove the upper water layer by separating, add 20mL of chloroform to dissolve the product in the collected organic layer, and then add 90mL of deionized water to the chlorofo...

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Abstract

The invention relates to the field of organic chemistry and aims to solve the problem that reaction conditions are harsh, the amount of byproducts is large, and the yield of a target product is low during preparation of an organic silicon polymer with an anthracene-protected alpha-cyanoacryloyloxy structure. The invention provides a preparation method of the organic silicon polymer with the anthracene-protected alpha-cyanoacryloyloxy structure. According to the method, gamma-chloropropyl silane and potassium anthracene-protected alpha-cyanoacrylate are taken as raw materials, and the organic silicon polymer with the anthracene-protected alpha-cyanoacryloyloxy structure is prepared by utilizing a condensation reaction. The preparation method has the advantages that energy consumption is low, environmental pollution is low, the method is safe and is friendly to the environment, the yield is high, products are easy to separate, the process and equipment are simple, production cost is low,and the like, and is suitable for industrial production.

Description

technical field [0001] The invention relates to the field of organic chemistry, in particular to a method for preparing an organosilicon compound containing an anthracene-protected α-cyanoacryloyloxy structure. Background technique [0002] Organosilicon compounds containing anthracene-protected α-cyanoacryloyloxy structures are important intermediates for the preparation of organosilicon compounds with α-cyanoacryloyloxy structures, which can undergo anionic polymerization under the action of moisture in the air Fast cross-linking and curing by means of fast cross-linking and curing, which endows silicone materials with the ability of fast cross-linking and curing under mild conditions, and is widely used in criminal investigation, intelligence collection, bonding, sealing, plugging and other fields that require rapid in-situ molding. [0003] There are few reports in the literature on the synthesis of small organosilicon compounds with anthracene-protected α-cyanoacryloylo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/08C07F7/18
CPCC07B2200/07C07F7/1892
Inventor 伍川邵方君董红瞿志荣苏丽吕叶红荣瑞蒋攀栾文耕蒋剑雄邱化玉
Owner HANGZHOU NORMAL UNIVERSITY
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