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Refining process of voglibose impurity n-methyl olamine

A technology based on methylenzyme olamine and voglibose, which is applied in the field of drug synthesis, can solve the problems of no published patents or literature reports, and achieve the effects of high efficiency, high purity and simple process

Active Publication Date: 2020-08-14
SHANDONG XINHUA PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] There are currently no published patents or literature reports

Method used

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  • Refining process of voglibose impurity n-methyl olamine
  • Refining process of voglibose impurity n-methyl olamine
  • Refining process of voglibose impurity n-methyl olamine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] First, react with iodomethane and the olamine of the enzyme olamine to obtain a crude product of N-methyl-olamine of the enzyme olamine with a content of about 30%.

[0034] Take 1g of crude product, absorb it with 80ml KY2-8 resin for half an hour, and then use 100ml H 2 O was eluted with 100ml MeOH / H 2 O=20% elution, then elution with 100ml pure MeOH, the obtained pure methanol eluent is mainly the target product N-methyl jinggangmycetin, and the obtained pure methanol eluent is concentrated to obtain N-methanol The crude product of base well gangase olamine has a purity of 80.22%.

[0035] In the second step, HPLC was used to prepare liquid phase separation, detected at 210 nm, eluted with 5% methanol, and the eluate of relatively pure target product was separated, concentrated, and freeze-dried to obtain 175 mg of N-methyl wellangase olamine with a content of 99.51%.

Embodiment 2

[0037] First, react with iodomethane and the olamine of the enzyme olamine to obtain a crude product of N-methyl-olamine of the enzyme olamine with a content of about 30%.

[0038] Take 1g of crude product, absorb it with 100ml 001×7 strongly acidic styrene-based cation exchange resin for half an hour, and then use 100ml H 2 O was eluted with 100ml MeOH / H 2 O=20% elution, then elution with 100ml pure MeOH, the obtained pure methanol eluent is mainly the target product N-methyl jinggangmycetin, and the obtained pure methanol eluent is concentrated to obtain N-methanol The crude product of base well gangase olamine has a purity of 85.56%.

[0039] In the second step, HPLC was used to prepare liquid phase separation, 210nm detection, 10% methanol elution, and the pure target product eluate was separated, concentrated, and freeze-dried to obtain 205 mg of N-methyl wellangase olamine with a content of 99.99%.

[0040] The proton nuclear magnetic spectrum, carbon nuclear magnetic ...

Embodiment 3

[0042] First, react with iodomethane and the olamine of the enzyme olamine to obtain a crude product of N-methyl-olamine of the enzyme olamine with a content of about 30%.

[0043] Take 1g of crude product, absorb it with 90ml Dowex50 resin for half an hour, then wash it with 100mlH 2 O was eluted with 100ml MeOH / H 2 O=20% elution, then elution with 100ml pure MeOH, the obtained pure methanol eluent is mainly the target product N-methyl jinggangmycetin, and the obtained pure methanol eluent is concentrated to obtain N-methanol The crude product of base well gangase olamine has a purity of 81.23%.

[0044] The second step adopts HPLC to prepare liquid phase separation, detect at 210nm, elute with 20% methanol, separate the eluate of relatively pure target product, concentrate, and freeze-dry to obtain 170 mg of N-methyl wellangase olamine with a content of 99.38%.

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Abstract

The invention relates to a refining technology of voglibose impurity N-methyl valiolamine. The refining technology comprises a two-step separation and purification method comprising the steps of (1) firstly adsorbing through a resin, and carrying out gradient elution, wherein a gradient elution process comprises H2O eluting, eluting according to MeOH / H2O being equal to 20 percent, and pure MeOH eluting; respectively obtaining three eluants through H2O eluting, eluting according to MeOH / H2O being equal to 20 percent, and pure MeOH eluting; (2) concentrating the pure MeOH eluant obtained in the(1) to obtain an N-methyl valiolamine crude product, adopting HPLC (High Performance Liquid Chromatography) for preparing a liquid phase, carrying out 210nm detection, eluting a methyl alcohol water solution, extracting an eluant, concentrating, and freeze-drying to obtain an N-methyl valiolamine pure product. The refining technology provided by the invention is simple in process, high in efficiency, high in purity, and capable of treating the N-methyl valiolamine crude product with the content being 30 percent through the treatment method so as to obtain the product with the purity being 99.9percent or more.

Description

technical field [0001] The invention relates to a process for refining voglibose impurity N-methyl olamine, which belongs to the technical field of medicine synthesis. Background technique [0002] Voglibose has an inhibitory effect on α-glucosidase, thereby inhibiting the hydrolysis of disaccharides and delaying the absorption of sugars. At the same time reduce hypertriglyceridemia and hyperinsulinemia. [0003] Voglibose has a remarkable hypoglycemic effect, and its market share in hypoglycemic drugs is getting higher and higher. It is necessary to study voglibose-related impurities, such as the impurity N-methyl olamine, during drug declaration. , to determine its effect on the in vivo activity of voglibose, so the study of voglibose impurities is very necessary. N-methyl oleic acid olamine is the degraded impurity of voglibose, also can produce in raw material storage process, the purpose of the present invention is to obtain more than 99.9% N-methyl lenic acid olamine...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C213/10C07C215/44
CPCC07B2200/07C07C213/10C07C215/44
Inventor 张富强常森
Owner SHANDONG XINHUA PHARMA CO LTD