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Preparation method of ceftriaxone sodium

A technology of ceftriaxone sodium and a system is applied in the field of preparation of ceftriaxone sodium, can solve the problems of high production cost, low product yield, pollution and the like, and achieves the effects of low production cost, simple production process and less waste water.

Inactive Publication Date: 2012-10-03
苏州盛达药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The preparation method of traditional ceftriaxone sodium mainly is in multi-solvent system, reacts by 7-ACT and AE-active ester under the effect of amine intermediate reactant, adds salt-forming agent and precipitates crystal again, and this synthetic route is long , high production cost, low product yield and serious pollution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] (1) Dissolve 20g of 7-ACA and 12g of triazine ring in 140ml of acetonitrile, cool down to below 10°C, add 120ml of boron trifluoride acetonitrile, fully stir and dissolve, control the temperature at 25~35°C for 1 hour, after the reaction Cool down, add 150ml of water, adjust with 20% sodium carbonate solution until the solution is turbid, grow crystals for 30min, and continue to adjust the pH value to 2.8~3.2. Stir slowly for 1 h and filter, separate the mother liquor, wash the crystals, and dry in vacuum at 45°C±2°C until qualified to obtain 24.6g of 7-ACT with a yield of 90.4%.

[0019] Add 25 g of potassium chloride to the separated mother liquor, stir at room temperature for 1 h to precipitate crystals, filter to obtain solid potassium fluoroborate for recovery, and recover acetonitrile in the filtrate.

[0020] (2) Add 20g of 7-ACT and 19g of AE-active ester to the reaction flask and dissolve in 100ml of dichloromethane solution, cool down to 0~5°C, add dropwise 15...

Embodiment 2

[0023] (1) Dissolve 20g of 7-ACA and 12g of triazine ring in 140ml of acetonitrile, cool down to below 10°C, add 120ml of boron trifluoride acetonitrile, fully stir and dissolve, control the temperature at 25~35°C for 1 hour, after the reaction Cool down, add 150ml of water, adjust with 20% sodium carbonate solution until the solution is turbid, grow crystals for 30min, and continue to adjust the pH value to 2.8~3.2. Stir slowly for 1 h and filter, separate the mother liquor, wash the crystals, and dry in vacuum at 45°C±2°C until qualified to obtain 24.6g of 7-ACT with a yield of 90.4%.

[0024] (2) Add 20g of 7-ACT and 19g of AE-active ester to the reaction flask, dissolve in 80ml of dichloromethane-20ml of methanol crystallization system, lower the temperature to 0~5°C, add dropwise 15ml of triethylamine in dichloromethane solution to react 5~6h, sampling HPLC method to measure 7-ACT residue. After passing the test, add water, separate phases, recover the organic phase, add...

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PUM

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Abstract

The invention discloses a preparation method of ceftriaxone sodium. The method comprises the following steps: with 7-ACA and triazine ring as raw materials, reacting under the catalysis of boron trifluoride acetonitrile, crystallizing to obtain 7-ACT, recovering potassium fluoborate and acetonitrile from the mother solution, dissolving 7-ACT and AE-active ester in a unitary or binary solvent system, reacting under catalysis of an organic base, adding a salifying agent and a water-soluble organic solvent in the water phase to separate out sodium salt and obtain ceftriaxone sodium, and recovering 2-mercaptobenzothiazole from the organic phase. The preparation method of ceftriaxone sodium provided by the invention has simple production process and low production cost, the yields in two steps are both higher than 90 percent, the solvents, organic matters, inorganic salts and the like in the reaction system can be recycled, and no or little waste water is generated.

Description

technical field [0001] The invention relates to the field of chemical pharmacy, in particular to a preparation method of ceftriaxone sodium. Background technique [0002] Ceftriaxone sodium, chemical name: (6R,7R)-7-[[(2-amino-4-thiazolyl)(methoxyimino)acetyl]amino]-8-oxo-3 -[[(1,2,5,6-tetrahydro-2-methyl-5,6-dioxo-1,2,4-triazin-3-yl)thio]methyl]-5- Thio-l-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid disodium salt triple hemihydrate. Ceftriaxone sodium is a third-generation cephalosporin antibiotic with broad-spectrum and high-efficiency characteristics. It is used for urinary tract, biliary tract infection, lower respiratory tract infection, pelvic infection, abdominal infection, bone and joint infection caused by sensitive pathogenic bacteria. Infection, skin and soft tissue infection, sepsis, meningitis and other diseases. [0003] The preparation method of traditional ceftriaxone sodium mainly is in multi-solvent system, reacts by 7-ACT and AE-active ester under the e...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/36C07D501/06
Inventor 张波周自金杨虎星温雄飞尹鸿冰吕德新
Owner 苏州盛达药业有限公司
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