Method for preparing vancomycin of norhydrochloric acid

A methyl vancomycin and hydrochloric acid technology, applied in the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., can solve the problems of norvancomycin degradation, poor appearance quality, long filtration time, etc. The effect of production cycle, reduced damage, and improved product yield

Active Publication Date: 2005-06-15
华北制药华胜有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] There are many deficiencies in this method, such as: the filtration time is long, and the filtration yield is low; the adoption of alkaline resolving agent can easily cause norvancomycin degradation, and the instant

Method used

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  • Method for preparing vancomycin of norhydrochloric acid
  • Method for preparing vancomycin of norhydrochloric acid
  • Method for preparing vancomycin of norhydrochloric acid

Examples

Experimental program
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Embodiment 1

[0028] Preparation of norvancomycin hydrochloride

[0029] Add 1~5% perlite (Henan Zhongnan Filter Aid Co., Ltd.), 2~13% potassium ferricyanide (commercially available product) and 2~10% zinc sulfate (commercially available) to norvancomycin fermented liquid product), stir evenly, plate and frame filter, and the filtrate passes through the column of macroporous decolorizing resin X-5 (Nankai University Resin Factory) with a flow rate of 1~2BV / hour, the unit of decolorizing solution is 3000~5000ug / ml, it is concentrated to 20000~30000ug / ml, the concentrated solution passes through the column of Sephadex G-10 resin (Nankai University Resin Factory) at a flow rate of 1~1.5BV / hour, and the saturated Sephadex G-10 resin uses 0.1mol / L Phosphoric acid aqueous solution elution, the elution rate is 0.5 ~ 1BV / hour, when HPLC detects that demethyl vancomycin hydrochloride flows out, start to collect, slowly add 0.5mol / L sodium hydroxide (commercially available product) aqueous solution t...

Embodiment 2

[0031] Preparation of norvancomycin hydrochloride

[0032] With embodiment 1, just the add-on of perlite is 3%, 7% potassium ferricyanide and 5% zinc sulfate, macroporous decolorizing resin is D941 (Nankai University Resin Factory), and the unit of decolorizing solution is 3672ug / ml, Concentrate it to 23500ug / ml, and the concentrated solution passes through the Sephadex G-15 resin column at a flow rate of 1BV / hour, and the saturated Sephadex G-15 resin is eluted with 0.1mol / L phosphoric acid aqueous solution, and the resolution rate 0.5BV / hour, the analytical solution was adjusted to pH 7.0-7.4 with 0.5mol / L sodium hydroxide aqueous solution, left to stand for 24 hours, plate and frame filtered, the filter cake was dissolved with 1% hydrochloric acid aqueous solution, and 5 times the volume of industrial acetone After crystallization, stand still for 24 hours, plate-and-frame filter press, wash, and vacuum-dry to obtain norvancomycin hydrochloride fine powder. The content of ...

Embodiment 3

[0034] Preparation of norvancomycin hydrochloride

[0035] With embodiment 1, just the add-on of perlite is 5%, 13% potassium ferricyanide and 2% zinc sulfate, use XAD-III macroporous decolorizing resin (Nankai University Resin Factory) decolorizing, the unit of decolorizing liquid is 4120ug / ml, it is concentrated to 27800ug / ml, the concentrated solution passes through the Sephadex G-25 resin column at a flow rate of 1BV / hour, and the saturated Sephadex G-25 resin is analyzed with 0.1mol / L hydrochloric acid aqueous solution, The analysis speed is 0.5BV / hour, the analysis solution is adjusted to pH 7.8 with 0.5mol / L sodium hydroxide aqueous solution, let stand for 24 hours, plate and frame filter, the filter cake is dissolved with 1% hydrochloric acid aqueous solution, and 10 times the volume of industrial acetone After crystallization, stand still for 24 hours, plate and frame press filter, wash, and vacuum-dry to obtain norvancomycin hydrochloride fine powder. The content o...

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Abstract

A process for preparing the norvancomycin hydrochloride includes such steps as proportionally adding pearlite, potassium ferricyanide and zinc sulfate to the fermented liquid of norvancomycin, stirring, filter, decoloring by macroreticular resin, absorbing by glucosal gel, acidic desorption, regulating pH-6.0-7.8, filter, dissolving the filtered cake in the aqueous solution of hydrochloric acid, crystallizing in acetone, and drying. Its advantages are high quality and output rate.

Description

technical field [0001] The invention relates to a preparation method of pharmaceutical raw materials, in particular to a preparation method of demethylvancomycin hydrochloride. Background technique [0002] Demethylvancomycin hydrochloride is a glycopeptide antibiotic with the following structural formula: [0003] [0004] The appearance of this product is light brown powder, odorless, bitter taste, soluble in water, slightly soluble in methanol, insoluble in acetone, butanol or ether, and can be precipitated by various heavy metal salts in the solution. [0005] Pharmacological and clinical studies in recent years have proved that desmethylvancomycin hydrochloride intravenous infusion is suitable for endocarditis, osteomyelitis, pneumonia, sepsis or soft tissue infection, etc. It is also used as the drug of choice for the treatment of enterococcal endocarditis and Corynebacterium (diphtheria-like genus) endocarditis in those who are allergic to penicillin. Treatment ...

Claims

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Application Information

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IPC IPC(8): C07H1/06C07H15/20
Inventor 姜杨张雪霞刘刚叁蒋沁修林坡李淑兰王琳张志江贺广峰
Owner 华北制药华胜有限公司
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