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A kind of non-dihydroxy monomethoxy polyethylene glycol and preparation method thereof

A technology of non-bishydroxyl monomethoxy and methoxypolyethylene glycol, applied in the field of bishydroxyl monomethoxypolyethylene glycol and its preparation

Active Publication Date: 2019-09-03
WENZHOU UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

A kind of preparation method of synthesizing non-bishydroxyl monomethoxy polyethylene glycol of the present invention can solve this problem, there is a kind of preparation method of synthesizing non-dihydroxy monomethoxy polyethylene glycol of the present invention at home and abroad No report

Method used

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  • A kind of non-dihydroxy monomethoxy polyethylene glycol and preparation method thereof
  • A kind of non-dihydroxy monomethoxy polyethylene glycol and preparation method thereof
  • A kind of non-dihydroxy monomethoxy polyethylene glycol and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Preparation of 2k-free double hydroxyl monomethoxy polyethylene glycol by reaction of vinyl glycol ether and ethylene oxide

[0023] Add 1.0g (0.011mol) of vinyl glycol ether, 5ml of DPMK (0.6mol / L), 30ml of tetrahydrofuran, and 21g of ethylene oxide into a dry and clean 300ml ampo bottle in sequence, and react at an oil bath temperature of 30-40°C 20-40min, then increase the temperature by 5-10°C every 20-40min until 60-70°C. Continue to react for 20-30h. After the reaction was completed, the temperature was lowered to normal temperature, 0.8g NaH was added, and stirred for 20-40min. Then add 6.45g iodomethane, react for 7-9h. Finally, hydrochloric acid aqueous solution was added to neutralize to a pH value of 5±1. After reacting for 4-8 hours, the product was obtained by purification and removal of impurities.

Embodiment 2

[0025] Preparation of 5k Polyethylene Glycol without Dihydroxy Monomethoxy by Reaction of Vinyl Glycol Ether and Ethylene Oxide

[0026] Add 0.4g (4.54mmol) of vinyl glycol ether, 2.5ml of DPMK (0.6mol / L), 35ml of tetrahydrofuran, and 22g of ethylene oxide into a dry and clean 350ml ampoule in sequence, and in an oil bath at a temperature of 30-40°C React for 20-40min, then raise the temperature by 5-10°C every 20-40min until 60-70°C. Continue to react for 20-30h. After the reaction was completed, the temperature was lowered to normal temperature, 0.35g NaH was added, and stirred for 20-40min. Then add 3.35g iodomethane, react for 7-9h. Finally, hydrochloric acid aqueous solution was added to neutralize to a pH value of 5±1. After reacting for 4-8 hours, the product was obtained by purification and removal of impurities.

Embodiment 3

[0028] Preparation of 2k-free double hydroxyl monomethoxy polyethylene glycol by reaction of 4-hydroxybutyl vinyl ether with ethylene oxide

[0029] Add 1g (8.6mmol) of 4-hydroxybutyl vinyl ether, 3.6ml of DPMK (0.6mol / L), 30ml of tetrahydrofuran, and 16g of ethylene oxide into a dry and clean 350ml ampo bottle in sequence, and put it in an oil bath at a temperature of 30-40°C React at low temperature for 20-40min, then raise the temperature by 5-10°C every 20-40min until 60-70°C. Continue to react for 20-30h. After the reaction was completed, the temperature was lowered to normal temperature, 0.69 g of NaH was added, and stirred for 20-40 min. Then add 4.9g iodomethane, react for 7-9h. Finally, hydrochloric acid aqueous solution was added to neutralize to a pH value of 5±1. After reacting for 4-8 hours, the product was obtained by purification and removal of impurities.

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Abstract

The invention discloses a mono-methoxyl polyethylene glycol without double hydroxyl groups and a preparation method thereof. The invention introduces a preparation method of synthesizing mono-methoxyl polyethylene glycol without double hydroxyl groups. According to the preparation method, 4-hydroxybutyl vinyl ether or vinyl glycol ether is taken as the initiator to synthesize methoxyl polyethylene glycol, then methanation of iodine is performed to block the terminal hydroxyl groups; and finally, a hydrochloric acid water solution with a pH value of 4-6 is used to remove the ether bonds of vinyl groups to obtain mono-methoxyl polyethylene glycol without double hydroxyl groups.

Description

technical field [0001] The invention belongs to the field of organic macromolecular chemistry, and specifically refers to non-bishydroxy monomethoxy polyethylene glycol and a preparation method thereof. Background technique [0002] Polyethylene oxide is a class of (—CH 2 CH 2 O—) is a polymer with a structural unit, and polyethylene glycol is widely used in the biomedical field because it has the following excellent properties: 1. The synthesis method is simple and controllable, and the terminal function can be obtained by anionic polymerization technology 2. The solubility in water is very good, and polyethylene glycol has high solubility in water, phosphate buffer solution, and normal saline; 3. The toxic and side effects on the human body are small, and polyethylene glycol is obtained by FDA approved for use as an additive or carrier in various pharmaceutical preparations. The toxicity of polyethylene glycol is very small, and there is no toxicity when it is administe...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/337C08G65/28
Inventor 李钟玉卢成洁王禄胜卢稳
Owner WENZHOU UNIVERSITY