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Catalyzing method of medecamycin

A midememycin and crystallization technology, applied in the new midemycin crystallization field, can solve the problems of reduced product content, high residual solvent, and high proportion data, and achieve the effect of reducing the impurity content of the finished product

Active Publication Date: 2015-06-17
NEW FOUNDER HLDG DEV LLC +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among the products obtained by the current crystallization process, this ratio data is relatively high and very unstable, ranging from 1:30 to 1:5;
[0007] 2. Residual solvents are high or require cumbersome processing to obtain qualified products;
[0008] 3. Because the crystallization process is water-phase crystallization, if the method of heating and drying is used for drying, hydrolytic damage will occur, resulting in a decrease in product content

Method used

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  • Catalyzing method of medecamycin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] Take 100g of midecamycin crude product with a content of 75.0%, add it to 300ml of isobutyraldehyde, heat to 50°C and stir until completely dissolved, then add 300ml of n-hexane dropwise under the condition of keeping warm at 50°C for 1 hour, and grow the crystal After 1 hour, control the cooling according to the cooling curve in the table below.

[0055] cooling time

[0056] The crystals were separated and vacuum-dried at 60-65° C. to constant weight to obtain 72.7 g of the finished product, the content of midecamycin was 88.3%, and the ratio of the absorption value at 280 nm to the absorption value at 232 nm was 1.87%.

Embodiment 2

[0058] Get content and be 75.0% midecamycin crude product 100g, add in the mixed solution of 250ml acetone and 50ml ethanol, add dropwise 300ml purified water under the condition of keeping warm at 20 ℃, the dropping rate is controlled in the mode described in the following table:

[0059] time

[0060] The crystals were separated and vacuum-dried at 35-40° C. to constant weight to obtain 70.3 g of the finished product, the content of midecamycin was 89.7%, and the ratio of 280nm absorption value to 232nm absorption value was 1.75%.

Embodiment 3

[0062] Take 100g of midecamycin crude product with a content of 75.0%, add 350ml of 2-octanone and 150ml of octane to the mixed solution, stir and dissolve at 60°C completely, cool down to -20°C at a rate of 5°C / hour, separate the crystals, and use The crystals were washed with 200ml of cyclohexane, and vacuum-dried at 35-40°C to constant weight to obtain 70.0g of finished product with a content of midecamycin of 88.7%. The ratio of the 280nm absorption value to the 232nm absorption value is 1.93%.

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Abstract

The invention provides a catalyzing method of medecamycin. The method comprises the following step of: crystalizing crude medecamycin with a mixed solvent to precipitate medecamycin out, wherein the mixed solvent comprises (1) a first solvent which is an aldehyde solvent with 1-6 carbon atoms or a solvent with 3-8 carbon atoms, and (2) a second solvent which is mutually soluble with the first solvent; and the solubility of the medecamycin in the first solvent is higher than the solubility of the medecamycin in the second solvent. The catalyzing method has the positive effects that: the impurity content of a finished product is lowered greatly, the content of organic solvents left in the finished product is low, and the content of medecamycin in the finished product is increased by over 10 percent than that before crystalizing.

Description

technical field [0001] The invention belongs to the field of pharmacy, and in particular relates to a new method for crystallizing midecamycin. Background technique [0002] Midecamycin is a sixteen-membered ring macrolide antibiotic, belonging to the macrolide multicomponent antibiotics, containing A 1 、A 2 、A 3 、A 4 four components. The main one used as medicine is the A 1 component, and its content should not be less than 75%. Midecamycin molecular structure is as shown in (I): [0003] where A 1 R=COCH in the component 2 CH 3 . [0004] [0005] The current crystallization method of midecamycin is as follows: enrich midecamycin in acidic aqueous solution through preliminary operations (the process may include: fermentation broth→filtration→organic solvent extraction→acid buffer into water), and then add alkali to it neutral solution. Since midecamycin has low water solubility under alkaline conditions, as the pH rises, midecamycin is gradually precipitated...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H17/08C07H1/06
Inventor 赵德易昆
Owner NEW FOUNDER HLDG DEV LLC