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Preparation method of high-purity polyethylene glycol diacrylamide

A technology of polyethylene glycol bisacrylamide and polyethylene glycol, applied in the field of preparation of high-purity polyethylene glycol bisacrylamide, can solve problems such as complicated operation, achieve high purity, accelerate reaction and improve yield. Effect

Active Publication Date: 2021-09-24
SHANGHAI YISIMIAO MEDICAL INSTR CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In order to solve the problems such as complicated operation in the above-mentioned prior art, the present invention provides a kind of preparation method of high-purity polyethylene glycol diacrylamide

Method used

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  • Preparation method of high-purity polyethylene glycol diacrylamide
  • Preparation method of high-purity polyethylene glycol diacrylamide
  • Preparation method of high-purity polyethylene glycol diacrylamide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Preparation of ethylene glycol mesylate

[0020]

[0021] Weigh 50g of PEG8000 into a 250ml three-neck flask, add 140ml of ethyl acetate, cool to 0-10°C in an ice-water bath with stirring, add 2.15ml of TEA, add 36mg of DMAP, stir for 10-30min, add 2.35ml of methanesulfonyl chloride, and naturally heat up to 25-35°C, stirred for 16-20h. Suction filter the reaction solution to remove insoluble impurities, add 300 ml of saturated saline, stir and wash, separate the liquids to obtain the DCM phase, dry and filter over anhydrous sodium sulfate, concentrate the filtrate under reduced pressure to a viscous state, pour 130 ml of tertiary methyl ether to precipitate, The solid was obtained by suction filtration, and dried in a vacuum oven at 35-50° C. to obtain 45 g of a white solid (ie, ethylene glycol mesylate).

[0022] Preparation of aminopolyethylene glycol

[0023]

[0024] Weigh 44.0g of the reactant obtained in the previous step into a 500ml three-necked fla...

Embodiment 2

[0029] The difference from Example 1 is that Preparation of aminopolyethylene glycol

[0030] Weigh 44.0g of the reaction product obtained in the previous step into a 500ml three-neck flask, add 400ml of ammonia water, add 1.4g of ammonium chloride and stir at room temperature for 1-2 days, add 400ml of DCM to the reaction solution, separate and collect the DCM phase, anhydrous sulfuric acid Sodium-dried and filtered with suction, the filtrate was concentrated under reduced pressure to thick, and 50ml of tertiary methyl ether was added to precipitate it. The solid was obtained by suction filtration, and dried in a vacuum oven at 35-50° C. to obtain 32 g of a white solid with a yield of 72.7% and a purity of 98.0%.

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Abstract

The invention relates to a preparation method of high-purity polyethylene glycol diacrylamide, and the reaction equation is shown in the specification, wherein n is equal to 1-350, ammonia water and ammonium chloride are sequentially added into polyethylene glycol methanesulfonate, and stirring reaction is performed at room temperature to obtain amino polyethylene glycol. According to the preparation method of the high-purity polyethylene glycol diacrylamide, ammonia gas in ammonia water is used as an ammonia reagent, sodium azide is avoided, ammonium chloride is added to accelerate the reaction and improve the yield, the reaction is safer and more controllable, and the preparation method is suitable for industrial production. Moreover, according to the preparation method disclosed by the invention, the purity of the obtained polyethylene glycol diacrylamide is relatively high, and the nuclear magnetic purity is greater than or equal to 99%.

Description

technical field [0001] The invention relates to high molecular polymers, more particularly to a preparation method of high-purity polyethylene glycol diacrylamide. Background technique [0002] Polyethylene glycol diacrylamide, as a polyethylene glycol polymer, is a polymer material widely used in the field of biomedicine. The existing preparation method of polyethylene glycol diacrylamide is either cumbersome to operate, or the purity of the obtained product is too low. Contents of the invention [0003] In order to solve the above-mentioned problems such as cumbersome operation in the prior art, the present invention provides a method for preparing high-purity polyethylene glycol diacrylamide. [0004] According to the preparation method of high-purity polyethylene glycol diacrylamide of the present invention, its reaction equation is as follows: [0005] , wherein n=1-350, wherein ammonia water and ammonium chloride are sequentially added to polyethylene glycol meth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/332C08G65/325C08G65/334
CPCC08G65/3322C08G65/3255C08G65/3346
Inventor 郭晓勇王翔刘翠钗
Owner SHANGHAI YISIMIAO MEDICAL INSTR CO LTD
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