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Furo urea penicillin sodium crystal and its synthesis

A technology of furacillin sodium and ampicillin acid, which is applied in the field of furacillin sodium crystal and its synthesis, can solve the problems of poor product stability, long synthesis route, many reaction and processing steps, etc., and achieve the reduction of solvent consumption, The effect of short production cycle and simple route

Inactive Publication Date: 2006-11-01
北京信汇科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are many deficiencies in this method: the synthesis route is relatively long, the reaction and treatment steps are more, a large amount of organic solvents are needed, a large amount of waste water is produced in the phase transfer process, the environment is polluted, and the reaction yield can only reach 60-70%
The synthesis steps are complicated, and the synthesis process is also carried out in the water phase, so phase transfer is also required, resulting in a large amount of waste water
And above-mentioned two kinds of methods all need to go through freeze-drying treatment, require high to equipment, and production cost is higher
[0006] It is shown by X-ray powder diffraction detection that the furosecillin sodium sold in the market is all amorphous furosecillin sodium, and the furosecillin sodium without crystal form has poor product stability
Although the iodine titration method is currently used (referring to the ministerial standard, Ministry of Health drug standard antibiotic drug (volume one) (1989), the standard number is WS 1 -C 2 -0021-89) measure the purity of the furosemide sodium sold on the market and all reached about 90%, but adopt more accurate high pressure liquid chromatography to detect the purity of above-mentioned furosemide penicillin sodium but can only reach 50-60% %

Method used

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  • Furo urea penicillin sodium crystal and its synthesis
  • Furo urea penicillin sodium crystal and its synthesis
  • Furo urea penicillin sodium crystal and its synthesis

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] Add 32 g of tetrahydrofuran into a 250 ml four-neck flask, stir and add 10 g of anhydrous ampicillin acid. Since anhydrous ampicillin acid is insoluble in tetrahydrofuran, the reaction solution is in a suspension state. The reaction system was cooled to -5°C to 10°C while stirring, and 4.3 g of 2-furanoyl isocyanate was added dropwise. The reaction solution gradually became clear to obtain a furosemide penicillin acid solution. Maintain the temperature at -5°C to 10°C, then add 5% sodium methoxide in isopropanol solution (every 100g of isopropanol contains 5 grams of sodium methoxide), until the pH of the reaction solution is 6.8, slowly in the reaction system A white crystalline substance, that is, crystals of furacillin sodium, was precipitated. After filtering, the filter cake was washed twice with isopropanol, sucked dry and dried below 60° C. to obtain 13.25 g of fururabenicillin sodium crystals with a yield of 91.03%. As detected by high-pressure liquid chromato...

Embodiment 2

[0071] Add 40 g of tetrahydrofuran into a 250 ml four-neck flask, stir and add 10 g of anhydrous ampicillin acid. Since anhydrous ampicillin acid is insoluble in tetrahydrofuran, the reaction solution is in a suspension state. While stirring, the reaction system was cooled to -5°C to 10°C, and 4.5 g of 2-furanoyl isocyanate was added dropwise. The reaction solution gradually became clear to obtain a furosemide penicillin acid solution. Then add 52 grams of isopropanol, maintain the temperature at -5°C to 5°C, then add 2% sodium methylate in isopropanol (every 100 grams of isopropanol contains 2 grams of sodium methylate), until the pH of the reaction solution was 6.8, and white crystals slowly precipitated out in the reaction system, i.e. fururabenicillin sodium crystals. After filtering, the filter cake was washed twice with isopropanol, sucked dry and dried at 50° C. to obtain 13.5 g of fururabenicillin sodium crystals with a yield of 93.0%. High pressure liquid chromatogr...

Embodiment 3

[0081] Add 40 g of tetrahydrofuran into a 250 ml four-neck flask, stir and add 10 g of anhydrous ampicillin acid. Since anhydrous ampicillin acid is insoluble in tetrahydrofuran, the reaction solution is in a suspension state. The reaction system was cooled to -5°C to 0°C while stirring, and 4.3 g of 2-furanoyl isocyanate was added dropwise. The reaction solution gradually became clear to obtain a furosemide penicillin acid solution. The reaction solution maintains a temperature of -5°C to 0°C, then adds 5% sodium methylate in dehydrated alcohol (every 100 grams of dehydrated ethanol contains 5 grams of sodium methoxide), until the pH of the reaction solution is 6.8, the reaction solution is carried out After the ethanol was removed under reduced pressure, the solid precipitated out, then dissolved with 95% ethanol, and 70 grams of isopropanol was used to separate out the crystals of furosecillin sodium, filtered and dried to obtain 13.3 grams of furosecillin sodium crystals, ...

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Abstract

Fuureidoparasiticin sodium crystal and its synthesis are disclosed. It is simple, has short production period, less organic solvent, more yield and higher crystal purity.

Description

technical field [0001] The present invention relates to a crystal of furacillin sodium and a synthesis method thereof. Background technique [0002] The chemical structural formula of fururacillin sodium is as follows: [0003] [0004] Furacillin sodium is a semi-synthetic penicillin, which has anti-negative bacteria, especially against Pseudomonas aeruginosa, meningococcus, Escherichia coli, Salmonella typhi and Proteus, etc., especially against Pseudomonas aeruginosa than carbenzyl It is several times stronger than piperacillin, and it is mainly used clinically for wound infection, sepsis, respiratory tract, urinary tract infection and other diseases, and has a wide range of uses. [0005] At present, there are mainly two kinds of synthetic methods of fururacillin sodium. The 655-656 page of " preparation method of pharmaceutical intermediate " first volume [M] in 2001 discloses the synthetic method of 2-(2-furoyl) ureidophenylacetic acid: 2-furoyl isocyanate (abbrev...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D499/46
Inventor 蒋征昊
Owner 北京信汇科技有限公司
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