Novel pulveres fosfomycin trometamol synthetic method

A technique for trometamol and tromethamine, which is applied in the field of synthesizing fosfomycin monotromethamine, can solve problems such as inappropriate rework, and achieve the effects of improving the production capacity of equipment and increasing the output of a single batch

Inactive Publication Date: 2004-11-10
NORTHEAST PHARMA GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Therefore, it is not appropriate to use water recrystallization for the rework of these unqualified products.

Method used

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  • Novel pulveres fosfomycin trometamol synthetic method
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  • Novel pulveres fosfomycin trometamol synthetic method

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Measure 70ml of anhydrous methanol and add it to a beaker containing 170ml of dry D001 cation exchange resin, stir evenly, then add the resin together with methanol to the exchange column with interlayer, open the low temperature bath, and lower the column temperature to - 20°C. Adjust the methanol liquid level in the column just slightly higher than the resin level, then add 14.5g of fosfomycin sodium (0.65% glycol) into the exchange column to start the exchange reaction, use anhydrous methanol as eluent, and continuously elute until there is no more fosfomycin acid flowing out from the bottom of the column, use about 600ml of anhydrous methanol, and directly add the eluted fosfomycin acid methanol solution into a 1000ml four-necked bottle filled with 8.6g tromethamine , carry out neutralization reaction, then add a small amount of activated carbon for decolorization for 10 minutes, filter, concentrate under reduced pressure to a liquid volume of 40-50ml, add 80ml of a...

Embodiment 2

[0032] Measure 100ml of anhydrous methanol into a beaker containing 220ml of dry D001 type cation exchange resin, stir evenly, then add the resin together with methanol into the exchange column with interlayer, open the low temperature bath, and lower the column temperature to - 17°C. Adjust the methanol liquid level in the column to be just slightly higher than the resin level, then add 14.5g of neutral fosfomycin sodium into the exchange column to start the exchange reaction, use anhydrous methanol as the eluent, and continue to elute until the bottom of the column is no longer Until fosfomycin acid flows out again, use about 650ml of anhydrous methanol to directly add the eluted fosfomycin acid methanol solution into a 1000ml four-neck bottle containing 26.0g fosfomycin bis tromethamine salt. Perform neutralization reaction, then add a small amount of activated carbon for decolorization for 10 minutes, filter, concentrate under reduced pressure to a liquid volume of 50-60ml...

Embodiment 3

[0036] Measure 50ml of anhydrous methanol and add it to a beaker containing 150ml of dry D001 cation exchange resin, stir evenly, then add the resin together with methanol to the exchange column with interlayer, open the low temperature bath, and lower the column temperature to - 14°C. Adjust the methanol liquid level in the column to be just slightly higher than the resin level, then add 14.5g of fosfomycin sodium (1.0% glycol) into the exchange column to start the exchange reaction, use anhydrous methanol as eluent, and continuously elute , until no more fosfomycin acid flows out from the bottom of the column, use about 600ml of anhydrous methanol, and directly add the eluted fosfomycin acid methanol solution to 1000ml of fosfomycin bis tromethamine salt containing 28g In a four-neck flask, carry out neutralization reaction, then add a small amount of activated carbon for decolorization for 10 minutes, filter, concentrate under reduced pressure to a liquid volume of 50-60ml,...

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Abstract

The invention provides a process for synthesizing pulveres fosfomycin trometamol by using phosphonomycin sodium or neutral phosphonomycin sodium containing small amount of organic acid as raw material through the steps of, subjecting 10-16 times of type H cationic ion-exchange resin to exchange reaction in methanol solution at low-temperature, with the methanol solution acting as eluent, thus preparing the methanol solution containing fosfomycin acid, neutralizing the methanol solution with right amount of tromethamine or fosfomycin methanol tromethamine salt so as to obtain the methanol solution of pulveres fosfomycin trometamol, and the end product of the methanol solution of pulveres fosfomycin trometamol is obtained from the methanol solution of pulveres fosfomycin trometamol from decolorizing, filtering, condensing, extracting, filtering and drying.

Description

1. Technical field: [0001] The invention provides a method for synthesizing fosfomycin monotromethamine using fosfomycin sodium or neutral fosfomycin sodium containing a small amount of organic acid as a raw material, which belongs to the field of fine chemical synthesis. 2. Background technology: [0002] Fosfomycin is a broad-spectrum, low-toxicity, non-sensitizing, non-sensitizing and resistant antibiotic that has a synergistic effect with most antibiotics. It was isolated from Spanish soil in 1966 by culturing Streptomyces freundii. The metabolites produced have inhibitory and killing effects on both Gram-positive and Gram-negative bacteria. Fosfomycin usually exists in the form of calcium salt and sodium salt, the calcium salt is used for oral administration, and the sodium salt is used for intravenous injection or drip. Sodium salt is divided into neutral fosfomycin sodium and basic fosfomycin sodium. In the production process of fosfomycin sodium and neutral fosfomy...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/655
Inventor 赵华
Owner NORTHEAST PHARMA GRP
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