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Preparation method of sulbactam acid

A technology of sulbactam acid and sulbactam sodium, which is applied in the field of preparation of pharmaceutical intermediates, can solve problems such as difficult product quality assurance, serious dust pollution of raw materials, complex synthesis reaction routes, etc. Good, high product content effect

Active Publication Date: 2018-12-14
NORTH CHINA PHARMA HEBEI HUAMIN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, the preparation methods of sulbactam acid disclosed in patent document CN101967155A and patent document CN102952147A are all synthetic reactions using 6-aminopenicillanic acid as a raw material. Serious, dark product color, many by-products, low yield and other problems, the product quality is difficult to be guaranteed

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0034] The invention discloses a preparation method of sulbactam acid, which uses sulbactam sodium as a raw material, and at the same time, adds a dissolving aid to a concentrated solution, and at the same time passes through carbon dioxide for crystallization to obtain sulbactam acid.

[0035] Sulbactam sodium is impurity, content, or any one or several of the indicators of color grade indicators that do not meet the quality standards, that is, total impurities > 1.0%, maximum single impurities > 0.5%, or color grade > No. 3; the concentrated solution is Sulbactam Tan sodium is obtained after dissolving, separating, decolorizing and concentrating.

[0036] The preparation method comprises the following steps:

[0037] A. Add 2 to 10 times of water to sulbactam sodium and stir until dissolved, add 2 to 12 times of the mass of sulbactam sodium in an organic solvent, adjust the pH to 0.5 to 2.5 with hydrochloric acid, sulfuric acid or phosphoric acid, and stir Stand to separate...

Embodiment 1

[0045] The invention discloses a preparation method of sulbactam acid, which uses sulbactam sodium as a raw material, and at the same time, adds a dissolving aid to a concentrated solution, and at the same time passes through carbon dioxide for crystallization to obtain sulbactam acid.

[0046] The preparation method comprises the following steps:

[0047] A. Add 60mL of purified water to 30g of sulbactam sodium (sulbactam sodium color grade No. 5) and stir until dissolved, then add 60mL of ethyl acetate, adjust the pH to 0.5 with hydrochloric acid, leave it to separate phases after stirring for 10min, and obtain A water phase and a solvent phase;

[0048] B. Add 150mL of ethyl acetate to the primary water phase, stir for 10min and then separate the phases to obtain a secondary water phase and a secondary solvent phase;

[0049] C. Combine the primary solvent phase and the secondary solvent phase, add 0.3 g of activated carbon, filter after stirring for 1 h, and wash with 30 ...

Embodiment 2

[0053] The invention discloses a preparation method of sulbactam acid, which uses sulbactam sodium as a raw material, and at the same time, adds a dissolving aid to a concentrated solution, and at the same time passes through carbon dioxide for crystallization to obtain sulbactam acid.

[0054] The preparation method comprises the following steps:

[0055] A. Add 300mL of purified water to 30g of sulbactam sodium (4.2% of the total impurities of sulbactam sodium, color grade No. 6) and stir until it dissolves, add the mixed solvent of 360mL ethyl acetate, butyl acetate and methyl acetate ( V:V:V=2:1:1), adjusted the pH to 2.5 with phosphoric acid, stirred for 10 minutes, and left to separate the phases to obtain a primary water phase and a primary solvent phase;

[0056] B. Add 90mL of a mixed solvent of ethyl acetate, butyl acetate and methyl acetate (V:V:V=2:1:1) to the primary water phase, stir for 10min and then stand to separate the phases to obtain the secondary water ph...

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PUM

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Abstract

The invention discloses a preparation method of sulbactam acid, and belongs to the field of preparation of pharmaceutical intermediates. The preparation method comprises the steps of: adopting sodiumsulbacetanate as a raw material, adding a dissolution-assistant agent to a concentrated liquid, introducing carbon dioxide at the same time, and performing crystallization so as to obtain sulbatam. Through the method, sodium sulbacetanate which does not meet the quality standard can be recycled and utilized fully, and the prepared sulbactam acid has the advantages of high content, less impurities,low color grade, good fluidity and good stability; and the preparation method is simple, energy-saving and environmentally friendly, and is suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to a preparation method of a compound, in particular to a preparation method of a β-lactam antibiotic intermediate, and belongs to the field of preparation of pharmaceutical intermediates. Background technique [0002] Sulbactamic acid is a white crystalline solid with the chemical name (2S,5R)-3,3-dimethyl-7-oxo-4-thia-1-azabicyclo[3,2,0]heptane Alkane-2-carboxylic acid-4,4-dioxide. Sulbactam acid is used to synthesize sulbactam sodium. It is a broad-spectrum β-lactamase inhibitor, which has a strong irreversible inhibitory effect on penicillinase and cephalosporinase. It is often combined with other β-lactams The combined use of antibiotics has obvious synergistic effect, which greatly improves the antibacterial activity and expands the antibacterial spectrum. The antibacterial activity against Staphylococcus, Catharella, Neisseria gonorrhoeae, Escherichia coli, Klebsiella, Haemophilus and Bacteroides is significantly enhanced...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D499/86C07D499/04C07D499/18
CPCC07D499/04C07D499/18C07D499/86
Inventor 田洪年贾全张锁庆石春利李庆伟刘树斌任峰贾金焕
Owner NORTH CHINA PHARMA HEBEI HUAMIN PHARMA
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