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Ceftriaxone sodium tetrahydrate compound

A technology of ceftriaxone sodium and its compound, which is applied in the field of ceftriaxone sodium tetrahydrate compound and its preparation method, and can solve the problems of increased production cost, waste of raw materials, instability between batches, etc.

Active Publication Date: 2019-01-04
陕西顿斯制药有限公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existence of these problems leads to poor product quality and instability between batches on the one hand, and also leads to increased production costs and waste of raw materials to a certain extent.

Method used

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  • Ceftriaxone sodium tetrahydrate compound
  • Ceftriaxone sodium tetrahydrate compound
  • Ceftriaxone sodium tetrahydrate compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1 4

[0035] The preparation of embodiment 1 ceftriaxone sodium tetrahydrate compound

[0036]Preparation Process:

[0037] (1) Slowly add 16.34g of sulfonyl chloride to 8.41g of dimethylformamide, stir well, add 100ml of dichloromethane, stir rapidly, slowly pour in 20.01g of aminothioxime acetic acid, and stir to obtain aminothiazide Clear solution of oxime acetic acid active.

[0038] (2) Add 35.10 g of 7-aminocefatriazine (7-ACT) into 200 ml of dichloromethane, stir well, cool, slowly add 20.01 g of tetramethylguanidine, and stir to obtain 7-ACT tetramethylguanidine salt solution.

[0039] (3) Add the activator solution of aminothioxime acetic acid into the solution of 7-ACT tetramethylguanidine salt for reaction. After adding 200ml of water, raise the temperature to 20°C, adjust the pH value to 6.0 with triethylamine, separate the water layer, add 1.50g of activated carbon and 0.55g of sodium bisulfite, decolorize for 30min, and filter. The filtrate was adjusted to pH 4.2 w...

Embodiment 2 4

[0045] The preparation of embodiment 2 ceftriaxone sodium tetrahydrate compound

[0046] Preparation Process:

[0047] (1) Slowly add 16.15g of sulfonyl chloride to 8.40g of dimethylformamide, stir evenly, add 100ml of dichloromethane, stir rapidly, slowly pour in 20.04g of aminothioxime acetic acid, and stir to obtain aminothiazide Clear solution of oxime acetic acid active.

[0048] (2) Add 35.10 g of 7-aminocefatriazine (7-ACT) into 200 ml of dichloromethane, stir well, cool, slowly add 20.00 g of tetramethylguanidine, and stir to obtain 7-ACT tetramethylguanidine salt The solution.

[0049] (3) Add the activator solution of aminothioxime acetic acid into the solution of 7-ACT tetramethylguanidine salt for reaction. After adding 200ml of water, raise the temperature to 25°C, adjust the pH value to 5.0 with triethylamine, separate the water layer, add 1.51g of activated carbon and 0.54g of sodium bisulfite, decolorize for 30min, and filter. The pH value of the filtrate w...

Embodiment 3 4

[0055] The preparation of embodiment 3 ceftriaxone sodium tetrahydrate compound

[0056] Preparation Process:

[0057] (1) Slowly add 16.21g of sulfonyl chloride to 8.47g of dimethylformamide, stir well, add 100ml of dichloromethane, stir rapidly, slowly pour in 20.08g of aminothioxime acetic acid, and stir to obtain aminothiazide Clear solution of oxime acetic acid active.

[0058] (2) Add 35.10 g of 7-aminocefatriazine (7-ACT) into 200 ml of dichloromethane, stir well, cool, slowly add 20.14 g of tetramethylguanidine, and stir to obtain 7-ACT tetramethylguanidine salt solution.

[0059] (3) Add the activator solution of aminothioxime acetic acid into the solution of 7-ACT tetramethylguanidine salt for reaction. After adding 200ml of water, raise the temperature to 15°C, adjust the pH value to 4.0 with triethylamine, separate the water layer, add 1.50g of activated carbon and 0.55g of sodium bisulfite, decolorize for 30min, and filter. The pH value of the filtrate was adj...

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Abstract

The invention discloses a ceftriaxone sodium tetrahydrate compound and a preparation method thereof. Each mole of ceftriaxone sodium contains four mole of water. According to the compound, sulfochlorides and dimethylformamide are adopted to be reacted to generate an activator, the activator is directly reacted with 7-aminoceftriazine tetramethylguanidine salt to obtain the ceftriaxone sodium tetrahydrate compound. The operation is simple, the obtaining of a reactant is easy, the reaction condition is milder, and the yield is high. The ceftriaxone sodium tetrahydrate compound has the advantagesof low hygroscopicity, low impurity content, good fluidity, good thermodynamic stability and more extensive application prospects.

Description

technical field [0001] The invention belongs to the technical field of chemical engineering medicine crystallization, and in particular relates to a ceftriaxone sodium tetrahydrate compound and a preparation method thereof. Background technique [0002] Ceftriaxone sodium (Ceftriaxone sodium) is a semi-synthetic third-generation cephalosporin drug, which was successfully developed by the Swiss company Roche in 1978. It was first listed in Switzerland in 1982 and obtained FDA certification in 1984. [0003] Compared with other cephalosporins, ceftriaxone sodium has the advantages of broad antibacterial spectrum, strong antibacterial effect, stability to β-lactamase, long blood half-life (7-9h), strong tissue penetration ability, less toxic and side effects, and good curative effect. . Clinically, it is mainly used for lower respiratory tract infection, urinary tract and biliary tract infection, abdominal infection, pelvic infection, sepsis, skin tissue infection, bone and jo...

Claims

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Application Information

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IPC IPC(8): C07D501/36C07D501/06A61K31/546A61P31/00
CPCC07B2200/13C07D501/06C07D501/36Y02A50/30
Inventor 王明
Owner 陕西顿斯制药有限公司
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