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Process for preparing ceftriaxone sodium

A ceftriaxone sodium and preparation process technology, applied in the field of compound preparation, can solve the problems of large solvent usage, high production cost, and long production cycle, and achieve the advantages of less solvent usage, low production cost, and short production cycle Effect

Inactive Publication Date: 2005-07-06
REYOUNG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Two-step process operation, the process uses a large amount of solvent, serious pollution, high labor intensity, long production cycle, high production cost, and low product yield

Method used

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  • Process for preparing ceftriaxone sodium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] The preparation technology of ceftriaxone sodium of the present invention is recorded as follows by operation time:

[0023] 7:30 Add 50ml of dichloromethane, 50ml of ethanol, 18ml of triethylamine, and 5ml of water into the three-necked bottle, stir and cool down under nitrogen protection;

[0024] 7:32 At 5°C, add 20g of 7-ACT, 20g of AE-active ester, and 0.5g of sodium bisulfite antioxidant:

[0025] 7:35 stirring reaction, temperature 6°C;

[0026] 9:30 The reaction was clarified, diluted with 30ml of ethanol, and filtered;

[0027] 9:45 Add sodium acetate aqueous solution dropwise;

[0028] 9:50 The solution is slightly muddy, add ceftriaxone sodium powder seed crystals to grow crystals;

[0029] 10:20 Add acetone dropwise to crystallize, share 400ml of acetone, temperature 10°C;

[0030] 11:50 Suction filtration to obtain a crystallization filter cake, washed with acetone;

[0031] 12:25 50 ℃ hot air drying;

[0032] 12:55 Drying is complete.

[0033] The d...

Embodiment 2

[0035] The preparation technology of ceftriaxone sodium of the present invention is as follows:

[0036] Add 50ml of dichloromethane, 50ml of ethanol, 18ml of triethylamine, and 5ml of water into a three-necked flask, stir and cool down under nitrogen protection until the temperature is 5°C, add 20g of 7-ACT, 20g of AE-active ester, and 0.5g of hydrogen sulfite Sodium antioxidant; stir until the reaction is clear, add 30ml of ethanol to dilute, filter; then add dropwise sodium acetate aqueous solution, the solution is slightly cloudy, add ftriaxone sodium powder seed crystals to grow crystals, then add dropwise acetone to crystallize, and suction filter to obtain crystals The filter cake was washed with acetone and dried to obtain the finished product.

Embodiment 3

[0038] The preparation technology of ceftriaxone sodium of the present invention is as follows:

[0039] Add 50ml of dichloromethane, 40ml of ethanol, 18ml of triethylamine, and 8ml of water into a three-neck flask, stir and cool down under nitrogen protection until the temperature is 8°C, add 20g of 7-ACT, 20g of AE-active ester, and 0.45g of bisulfite Sodium antioxidant; stir until the reaction is clear, add 35ml of ethanol to dilute, filter; then add dropwise sodium acetate aqueous solution, the solution is slightly cloudy, add ftriaxone sodium powder seed crystals to grow crystals, then add dropwise acetone to crystallize, and suction filter to obtain crystals The filter cake was washed with acetone and dried to obtain the finished product.

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Abstract

Disclosed is a process for preparing ceftriaxone sodium belonging to compound preparation technical field. Protected by nitrogen, 7-ACT3 reacts with AE-active ester under the action of amine intermediate reactant in a solvent. Then a sodium salt forming agent is added in, and the cefotaxime sodium is obtained after reaction and seedout. The solvent is a mixed solvent composed of alkane halocarbon, ethyl acetate, or acetone and alcohol solvent and water. The solvent dosage is small, and the product yield is high.

Description

technical field [0001] The invention relates to a preparation process of ceftriaxone sodium, which belongs to the technical field of compound preparation. Background technique [0002] Ceftriaxone sodium is a third-generation broad-spectrum cephalosporin, which is widely used in respiratory tract infections and urinary system infections sensitive to this product, including pyelonephritis and gonorrhea, sepsis, meningitis, burn infections, postoperative infections, bone Joint, soft tissue, skin and wound infection, abdominal infection (peritonitis, bile duct and gastrointestinal tract infection) and infection prevention during surgery. Existing ceftriaxone sodium preparation process is operated in two steps, protected by nitrogen, in dichloromethane single solvent, by 7-ACT and AE-active ester under the effect of triethylamine intermediate reactant (i.e. condensation agent) Carry out the reaction, then add hydrochloric acid to the reaction solution, stir and extract to obtai...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/36
Inventor 赵玉山苗得足刘伟孙霁红吕含富
Owner REYOUNG PHARMA
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