Refining method for piperacillin sodium

A piperacillin sodium and refining method technology, applied in the field of polymer removal, can solve the problems of high equipment cost, large solvent volume, cumbersome operation, etc., and achieve the effect of low production cost, simple operation and good refining effect

Active Publication Date: 2012-12-05
JIANGSU CAREFREE PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Mainly use ion-exchange column to adsorb impurities with large molecular weight and high polarity, and elute with methanol water. This method is cumbersome to operate, high in equipment cost, and takes a long time and a large amount of solvent in the elution process.

Method used

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  • Refining method for piperacillin sodium
  • Refining method for piperacillin sodium

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0020] The preparation method of piperacillin sodium crude product is as follows:

[0021] 1. In a dry reactor, add 7kg (49mol) of dioxypiperazine and 45L of dichloromethane, cool to -10°C, add 6.4kg (59mol) of trimethylchlorosilane, and add 6.0kg of triethylamine dropwise at the same temperature kg (59mol), reacted for 2 hours after dropping, and the solution was pale yellow. Then cool to -20°C, add 5.3 kg (18 mol) of triphosgene in batches, and react for 3 hours, the reaction solution changes from light yellow to light red. Filter and use the filtrate for later use.

[0022] 2. In a dry reaction kettle, add 150 L of dichloromethane, 16 kg (40 mol) of ampicillin trihydrate, and drop triethylamine to dissolve and clarify the solid. Add the above-mentioned steps to obtain the acid chloride solution in the product, and keep warm for reaction after adding. Add 3 mol / L HCl dropwise to acidify, adjust pH=1.5-2.0, let stand to separate layers, and discard the water layer. 250 L ...

example 1

[0024] The refining of example 1 piperacillin sodium crude product

[0025] Add 15.00kg of crude piperacillin sodium into 15L of water and 30L of DMSO, stir at 50°C to fully dissolve; add 1.5kg of activated carbon, stir well and filter while hot; add 75L of acetone dropwise to the filtrate; Room temperature; transfer to 5-10°C for 3 hours of heat preservation, stirring and crystallization; filter the filter cake and rinse with 1L of ice acetone; dry to obtain 11.85kg of refined piperacillin sodium, the polymer content of which is 0.09% as detected by HPLC.

example 2

[0026] The refining of example 2 piperacillin sodium crude product

[0027] Add 15.00kg of crude piperacillin sodium into 15L of water and 30L of DMSO, stir and fully dissolve at 50°C; add 1.5kg of activated carbon, stir well and filter while hot; add 150L of acetone dropwise to the filtrate; naturally cool down to room temperature while stirring ; Transfer to -10 ~ -5 ℃ heat preservation, stirring and crystallization for 5 hours; filter the filter cake and rinse with 1L of ice acetone; dry to obtain 12.30kg of piperacillin sodium refined product, the polymer content of HPLC is 0.08%.

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Abstract

The invention discloses a refining method for a piperacillin sodium crude product, wherein the method is mainly a method for removing polymers in the crude product. The method is performed according to the following steps: heating a piperacillin sodium crude product, and dissolving in water and DMSO; carrying out a treatment with active carbon; filtering; adding acetone in a dropwise manner; cooling; carrying out thermal insulation crystallization; and filtering to obtain the piperacillin sodium refined product. Compared with the polymer removing method and other methods reported in traditional literatures, the method of the present invention has characteristics of simple operation, low production cost, and high finished product purity, and can be used for industrial purification production of piperacillin sodium crude products, wherein the method reported in the traditional literatures adopts an ion exchange manner.

Description

technical field [0001] The invention relates to a refining method of crude piperacillin sodium, in particular to a method for removing polymers. technical background [0002] Piperacillin sodium (piperacilin sodium), the chemical name is (2S, 5R, 6R)-6-[2-(2R)-4-(4-ethyl-2,3-dioxo-1-piperazinyl) ) Sodium formamido-2-phenylacetamido] penicillanate. Structural formula: [0003] [0004] This product is developed by Japan Toyama Chemical Industry Co., Ltd. It is clinically applicable to sepsis caused by sensitive Enterobacteriaceae bacteria, Pseudomonas aeruginosa, Acinetobacter, upper urinary tract and complicated urinary tract infection, respiratory tract infection, and biliary tract infection , abdominal infection, pelvic infection, and skin and soft tissue infection. The combination of piperacillin sodium / sulbactam sodium and piperacillin sodium / tazobactam sodium has good stability, and shows strong antibacterial activity against common clinical enzyme-producing bacte...

Claims

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Application Information

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IPC IPC(8): C07D499/68C07D499/18
Inventor 秦引林
Owner JIANGSU CAREFREE PHARM CO LTD
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