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Mono-methoxyl polyethylene glycol without double hydroxyl groups and preparation method thereof

A technology without double hydroxyl monomethoxy and polyethylene glycol, applied in the field of double hydroxyl monomethoxy polyethylene glycol and its preparation

Active Publication Date: 2017-09-22
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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  • Mono-methoxyl polyethylene glycol without double hydroxyl groups and preparation method thereof
  • Mono-methoxyl polyethylene glycol without double hydroxyl groups and preparation method thereof
  • Mono-methoxyl polyethylene glycol without double hydroxyl groups and preparation method thereof

Examples

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Embodiment 1

[0022] Preparation of 2k non-bihydroxy monomethoxy polyethylene glycol synthesized by reaction of vinyl glycol ether and ethylene oxide

[0023] Add 1.0g (0.011mol) vinyl glycol ether, 5ml DPMK (0.6mol / L), 30ml tetrahydrofuran, 21g ethylene oxide into a dry and clean 300ml ampoule, and react at an oil bath temperature of 30-40℃ 20-40min, then increase the temperature by 5-10℃ every 20-40min until 60-70℃. Continue the reaction for 20-30h. After the reaction is completed, the temperature is reduced to room temperature, 0.8 g of NaH is added, and the mixture is stirred for 20-40 min. Then add 6.45g methyl iodide and react for 7-9h. Finally, an aqueous solution of hydrochloric acid was added to neutralize the pH to 5±1 and reacted for 4-8 hours, and the product was purified and removed.

Embodiment 2

[0025] Preparation of 5k non-dihydroxy monomethoxy polyethylene glycol synthesized 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, at an oil bath temperature of 30-40℃ React for 20-40 minutes, and then increase the temperature by 5-10°C every 20-40 minutes until 60-70°C. Continue the reaction for 20-30h. After the reaction is completed, the temperature is reduced to normal temperature, 0.35g NaH is added, and the mixture is stirred for 20-40 min. Then add 3.35g methyl iodide and react for 7-9h. Finally, an aqueous solution of hydrochloric acid was added to neutralize the pH to 5±1 and reacted for 4-8 hours, and the product was purified and removed.

Embodiment 3

[0028] Preparation of 2k non-bihydroxy monomethoxy polyethylene glycol synthesized by reaction of 4-hydroxybutyl vinyl ether and 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 ampoule in turn, at an oil bath temperature of 30-40℃ React for 20-40 minutes, and then increase the temperature by 5-10°C every 20-40 minutes until 60-70°C. Continue the reaction for 20-30h. After the reaction is completed, the temperature is reduced to room temperature, 0.69g NaH is added, and the mixture is stirred for 20-40 min. Then add 4.9g methyl iodide and react for 7-9h. Finally, an aqueous solution of hydrochloric acid was added to neutralize the pH to 5±1 and reacted for 4-8 hours, and the product was purified and removed.

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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 polymer chemistry, and specifically refers to non-dihydroxy monomethoxy polyethylene glycol and a preparation method thereof. Background technique [0002] Polyethylene oxide is a class with (—CH 2 CH 2 O—) is a structural unit polymer. Polyethylene glycol has a very wide range of applications in the field of biomedicine, because it has the following excellent properties: 1. The synthesis method is simple and controllable, and the terminal function can be obtained through anionic polymerization technology. 2. The solubility in water is very good. Polyethylene glycol has high solubility in water, phosphate buffer solution and physiological saline; 3. It has little toxic and side effects to the human body. FDA approved to be used as a variety of pharmaceutical additives or carriers. Polyethylene glycol is very toxic, and it is not toxic when it is taken orally, intravenously or administered through the skin with ...

Claims

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Application Information

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IPC IPC(8): C08G65/337C08G65/28
Inventor 李钟玉卢成洁王禄胜卢稳
Owner WENZHOU UNIVERSITY