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High-purity cefmenoxime hydrochloride compound

A technology of cefmenoxime hydrochloride and a compound, which is applied in the field of medicine, can solve the problems affecting the quality of preparations, poor color, poor purity, etc., and achieves the effects of optimizing product quality, simple process and improving purity

Inactive Publication Date: 2010-08-11
HAINAN LINGKANG PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] At present, the domestic preparation manufacturers of cefmenoxime hydrochloride mainly rely on imported raw materials, but its purity is poor, its color is not good, and its content is low, which affects the quality of its preparations. Therefore, a high-purity, high-content cefmenoxime hydrochloride Oxime has certain social and economic benefits

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] The refining of embodiment 1 cefmenoxime hydrochloride

[0018] (1) 100g of cefmenoxime hydrochloride crude product is dissolved in 120ml of water, then slowly add 5% sodium carbonate solution, stir to react to solution pH and be 7, then add the gac of 1.22g, stir at room temperature for 30 minutes, decarburize by filtration, collect filtrate.

[0019] (2) Add 0.1mol / L hydrochloric acid to the filtrate obtained in the upward step to react until the pH value of the solution is 5.5, then add 1000ml of isopropanol, stir and react at room temperature for 30 minutes, filter, and dry under reduced pressure at 45°C to obtain refined cephalosporin hydrochloride 91.4 g of methyloxime, the yield is 91.4%, and the HPLC purity is 99.6%.

[0020] 1 H-NMR MHz(Bruker AV400mHz)(DMSO-d 6 )δ: 9.63(d, 1H, CONH), 6.73(s, 1H, thiazole ring C 5 -H), 5.77 (dd, 1H, C 7 -H), 5.11(d, 1H, C 6 -H), 4.22(q, 2H, C 3 -CH 2 ), 3.93 (s, 3H, -OCH 3 ), 3.84 (s, 3H, -NCH 3 ), 3.72(q, 2H, C 2 -C...

Embodiment 2

[0021] The refining of embodiment 2 cefmenoxime hydrochloride

[0022] (1) 100g cefmenoxime hydrochloride crude product is dissolved in 150ml water, then slowly add 10% sodium bicarbonate solution, stirring reaction is 8 to solution pH, then adds the gac of 2.98g, stirs at room temperature 20 minutes, filter decarburization, Collect the filtrate.

[0023] (2) Add 1 mol / L hydrochloric acid to the filtrate obtained in the upward step to react until the pH value of the solution is 4.5, then add 150 ml of isopropanol, stir and react at room temperature for 60 minutes, filter, and dry under reduced pressure at 50 ° C to obtain refined cephalexin hydrochloride Oxime 92.5g, yield 92.5%, HPLC purity 99.5%.

[0024] 1 H-NMR MHz(Bruker AV400mHz)(DMSO-d 6 )δ: 9.63(d, 1H, CONH), 6.73(s, 1H, thiazole ring C 5 -H), 5.77 (dd, 1H, C 7 -H), 5.11(d, 1H, C 6 -H), 4.22(q, 2H, C 3 -CH 2 ), 3.93 (s, 3H, -OCH 3 ), 3.84 (s, 3H, -NCH 3 ), 3.72(q, 2H, C 2 -CH 2 ).

Embodiment 3

[0025] The refining of embodiment 3 cefmenoxime hydrochloride

[0026] (1) 100g cefmenoxime hydrochloride crude product is dissolved in 150ml water, then slowly add 8% sodium hydroxide solution, stirring reaction is 7.5 to solution pH, then adds the gac of 2.56g, stirs at room temperature 30 minutes, filter decarburization, Collect the filtrate.

[0027] (2) Add 0.5mol / L hydrochloric acid to the filtrate obtained in the upward step to react until the pH value of the solution is 5.0, then add 150ml of isopropanol, stir and react at room temperature for 60 minutes, filter, and dry under reduced pressure at 45°C to obtain refined cephalosporin hydrochloride Methyloxime 91.8g, the yield is 91.8%, and the HPLC purity is 99.6%.

[0028] 1 H-NMR MHz(Bruker AV400mHz)(DMSO-d 6 )δ: 9.63(d, 1H, CONH), 6.73(s, 1H, thiazole ring C 5 -H), 5.77 (dd, 1H, C 7 -H), 5.11(d, 1H, C 6 -H), 4.22(q, 2H, C 3 -CH 2 ), 3.93 (s, 3H, -OCH 3 ), 3.84 (s, 3H, -NCH 3 ), 3.72(q, 2H, C 2 -CH 2 ).

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Abstract

The invention relates to a cefmenoxime hydrochloride compound, which is prepared through acid-base reaction, activated carbon adsorption, separation and purification of prepared chromatography so as to achieve the aim of purification and obtain the high-purity cefmenoxime hydrochloride compound finally. The invention optimizes the product quality, and guarantees safety of clinical medication.

Description

technical field [0001] The invention relates to a method for purifying cefmenoxime hydrochloride compound. High-purity cefmenoxime hydrochloride can be obtained through the method of the invention, which belongs to the technical field of medicine. Background technique [0002] Cefmenoxime hydrochloride, its chemical name is: (6R, 7R)-7-[(Z)-2-(2-amino-4-thiazolyl)-2-methoxyiminoacetamido]-3-[[ 1-Methyl-1H-tetrazol-5-yl)-thio]methyl]-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-metha Hydrochloride (2:1), molecular formula: C 16 h 17 N 9 o 5 S 3 1 / 2HCl, molecular weight: 529.79, structural formula: [0003] [0004] Cefmenoxime hydrochloride is the third-generation cephalosporin developed by Takeda Corporation of Japan. It was first listed in Japan in 1983. It is a broad-spectrum antibiotic that achieves bactericidal effect by inhibiting the biosynthesis of bacterial cell walls. [0005] Regarding the synthetic method of cefmenoxime hydrochloride, according to literat...

Claims

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Application Information

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IPC IPC(8): C07D501/36C07D501/12
Inventor 陶灵刚
Owner HAINAN LINGKANG PHARMA CO LTD
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