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Method for purifying polyethylene glycol monomethyl ether monophosphate/diphosphate

A polyethylene glycol monomethyl ether and purification method technology, which is applied in the field of biomedicine, can solve problems such as difficulty in large-scale production, and achieve the effect of being easy to obtain and meeting the market's large-volume demand

Pending Publication Date: 2021-05-07
苏州欣影生物医药技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The technical problem to be solved by the present invention is to overcome the defects of the prior art, provide a method for purifying mono / bisphosphate polyethylene glycol monomethyl ether, reduce the cost required for purifying mono / bisphosphate polyethylene glycol monomethyl ether, Solve problems that are difficult to mass-produce

Method used

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  • Method for purifying polyethylene glycol monomethyl ether monophosphate/diphosphate

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Self-made polyethylene glycol monomethyl diphosphate 2.0g (purity HPLC: 93.7%), add 10ml of purified water to dissolve, adjust to alkaline with 10% NaOH aqueous solution, T=20~30℃, stir for 5min, the pH value is not Change again, add MeOH, THF, and DCM while stirring, stir at room temperature for 10 min, and let stand to separate layers. Separate the organic phase for waste liquid treatment, the water phase is the product, concentrate the water phase to dryness with a rotary evaporator, add MTBE, stir and crystallize for 30 minutes, filter to obtain the product solid, dry 1.63g, yield 77%, purity HPLC: 99.52% .

Embodiment 2

[0022] Self-made polyethylene glycol monomethyl diphosphate 2.0g (purity HPLC: 93.7%), add 10ml of purified water to dissolve, adjust to alkaline with 10% NaOH aqueous solution, T=20~30℃, stir for 5min, the pH value is not Change again, add methanol, dichloromethane and acetonitrile under stirring state, stir for 10 min, and let stand to separate layers. The organic phase was separated and treated as waste liquid, the aqueous phase was the product, the solvent was concentrated to dryness by a rotary evaporator, MTBE was added to stir and crystallize for 30 minutes, the product solid was obtained by filtration, and dried 1.67g, the yield was 79%, and the purity by HPLC: 99.67%.

Embodiment 3

[0024] Self-made polyethylene glycol monomethyl diphosphate 2.0g (purity HPLC: 93.7%), add 10ml of purified water to dissolve, adjust to alkaline with 10% NaOH aqueous solution, T=20~30℃, stir for 5min, the pH value is not Change again, add 2-methyltetrahydrofuran, dichloromethane and methanol mixed solvent under stirring state, stir for 10 min, and let stand to separate layers. Separate the organic phase for waste treatment, the water phase is the product, concentrate the solvent to dryness with a rotary evaporator, add 20ml of MTBE, stir and crystallize for 30min, filter to obtain the product solid, dry 1.71g, yield 81%, purity HPLC: 99.09% .

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Abstract

The invention discloses a method for purifying polyethylene glycol monomethyl ether monophosphate / diphosphate, and the method comprises the following steps: converting polyethylene glycol monomethyl ether monophosphate / diphosphate into a salt form by using alkali, and extracting impurities in a product from the product by using an organic solvent. The acidity of diphosphate groups of the product is utilized, and alkali is used for converting the diphosphate groups into salt, so that the water solubility of the diphosphate groups is better; most impurities in the crude product are olefin or amine derivatives, and are extracted from the product by using an organic solvent. According to the method, the polyethylene glycol monomethyl ether monophosphate / diphosphate with the purity of about 90% can be purified to 99% or above, required instruments, equipment and reagents are common and easy to obtain, large precise expensive instruments are not needed, and the process is simple and easy to operate. Large-scale production can be achieved, and the market large-scale requirement is met.

Description

technical field [0001] The invention relates to a method for purifying mono / diphosphate polyethylene glycol monomethyl ether, which belongs to the technical field of biomedicine. Background technique [0002] As a synthetic polymer material, polyethylene glycol is widely used in the field of medicine because of its good biological, blood compatibility and hydrophilicity, and no toxic and side effects. At present, the main research in drug modification is methoxypolyethylene glycol with an active terminal hydroxyl group. However, the activity of the terminal hydroxyl group of methoxypolyethylene glycol is weak and it is difficult to meet the needs of drug modification. The hydroxyl groups are transformed into more active groups such as amino groups, mercapto groups, and aldehyde groups for use. Mono / diphosphopolyethylene glycol monomethyl ether is widely used in various proteins, peptides and nanomedicines due to its excellent activity and adsorption properties of the end gr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/30
CPCC08G65/30
Inventor 孙江逵黄永娟薛文高明远肖陈华
Owner 苏州欣影生物医药技术有限公司
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