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Preparation method of high-purity ethyl 2-(2-aminothiazol-4-yl)-2-hydroxyiminoacetat

A high-purity technology for norfoxamic acid ethyl ester, which is applied to the preparation field of high-purity norfoxamic acid ethyl ester, can solve the problem of high production cost and achieve the effects of low cost, high yield and improved purity

Inactive Publication Date: 2019-01-04
SHANDONG JINCHENG PHARMACCUTICAL CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Patent CN200710013072 synthesized demethylaminothiaxate ethyl ester HPLC purity is only 98.5-98.8%, the impurity content is relatively high; patent CN201611253427 synthesized demethylaminothiaxate ethyl ester although the purity is high, but the production process needs to use a large amount of raw materials such as bromine and AMP , higher production cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Add 40 g of the crude product of ethyl demethylthioxamate (purity 97.1%, impurity 2.9%), add 53 L of tap water, 110 L of methanol, add hydrochloric acid dropwise to pH 1.0 at 31 ° C, the reaction temperature is 40 ° C, the time for acid adjustment is 12 min, after dissolving, add activated carbon 1.5 g, sodium pyrosulfite 1.0g, stirred at 31°C for 10min, raised the temperature to 35°C and filtered activated carbon, added dropwise triethylamine to the filtrate to pH 5.5, added dropwise for 33min, kept at 26°C for 30min, cooled to 5°C and filtered to obtain demethylaminothioxamic acid The refined ethyl ester has a purity of 99.92% and an impurity of 0.08%.

Embodiment 2

[0031] Add 40 g of the crude product of ethyl demethylaminothioxamate (purity 97.3%, impurity 2.6%), add 50 L of tap water, 110 L of ethanol, add hydrochloric acid dropwise to pH 1.5 at 28 ° C, the reaction temperature is 37 ° C, the time for acid adjustment is 15 min, after dissolving, add activated carbon 1.5 g, sodium bisulfite 1.0g, stir at 33°C for 10min, heat up to 40°C to filter activated carbon, take the filtrate and add N,N-dimethylaniline dropwise to pH 5.5, add dropwise for 30min, keep warm at 35°C for 30min, cool down to 8 ° C rejection filtration to obtain the refined product of ethyl demethylaminothiaxate with a purity of 99.90% and impurities of 0.10%.

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Abstract

The invention belongs to the technical field of pharmaceutical synthesis, and particularly relates to a preparation method of high-purity ethyl 2-(2-aminothiazol-4-yl)-2-hydroxyiminoacetat. The preparation method includes: adding a mixed solvent into a crude product of ethyl 2-(2-aminothiazol-4-yl)-2-hydroxyiminoacetat, heating up and stirring at a preserved temperature; adding hydrochloric acid to adjust systemic pH (potential of hydrogen), after the system dissolves clearly, adding activated carbon and a reducing agent, and stirring; filtering off the activated carbon, adjusting systemic pHof a filter liquor at 4.5-6.5 with organic alkali, and performing thermal reaction; cooling and spin-filtering to obtain competitive ethyl 2-(2-aminothiazol-4-yl)-2-hydroxyiminoacetat products. The preparation method of the high-purity ethyl 2-(2-aminothiazol-4-yl)-2-hydroxyiminoacetat has the advantages that the process is simple, purity of the ethyl 2-(2-aminothiazol-4-yl)-2-hydroxyiminoacetat is improved effectively and is above 99.85%, and product quality is optimized, and the preparation method is low in cost, high in yield and suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of medicine synthesis, and in particular relates to a preparation method of high-purity ethyl demethylthiaxamate. Background technique [0002] Ethyl demethylthioxamate is mainly used in the synthesis of cephalosporin antibiotics. It is an important side chain intermediate for the synthesis of β-lactam antibiotics cefixime, ceftiazole, ceftriaxone, ceftazidime, and cefpirome. It is a very promising One of the promising high value-added pharmaceutical intermediates. This type of drug has broad-spectrum antibacterial activity, has a significant effect on severe infections such as sepsis, meningitis, and pneumonia, and is basically non-toxic to the kidneys. It is an important antibiotic drug used in clinical treatment of infectious diseases. [0003] At present, the synthesized ethyl desmethiaxate has a darker appearance, and the market has higher and higher requirements for the purity of ethyl desmethiaxate, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D277/593
CPCC07D277/593
Inventor 孙兴李佳董玉龙赵文勇王瑞
Owner SHANDONG JINCHENG PHARMACCUTICAL CHEM CO LTD
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