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Lomefloxacin aspartate hydrate and its novel preparation method and use

A technology of lomefloxacin aspartate and lomefloxacin hydrochloride, which is applied in the field of medicine, can solve the problems of difficult to obtain and unfavorable hydrate preparation, quality control, and purification of lomefloxacin aspartate, and achieves Good dissolution properties, improved bioavailability, good storage stability

Inactive Publication Date: 2012-09-12
胡梨芳
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] The literature only reported lomefloxacin aspart [C 17 h 19 f 2 N 3 o 3 ·C 4 h 7 NO 4 , Molecular weight: 484.46] and its use as well as the hydrate of lomefloxacin aspartate and its preparation method, but the patent used lomefloxacin base when preparing the hydrate of lomefloxacin aspartate, the starting material The base is difficult to obtain, expensive, and the purification is troublesome, which is not conducive to the preparation and quality control of the hydrate of lomefloxacin aspartate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041]Example 1 In a three-necked flask, take 10 g of lomefloxacin hydrochloride and equimolar L-aspartic acid, dissolve lomefloxacin hydrochloride in water, and adjust the pH value to about 7 with 1M sodium hydroxide solution under stirring , add equimolar L-aspartic acid, stir to dissolve, let it stand for 1 hour, filter, slowly add 80ml of absolute ethanol to the filtrate, cool to below 0°C, wait for the solid to precipitate, filter, and rinse the solid with ethanol Several times, drained, recrystallized with an appropriate amount of ethanol water, filtered under reduced pressure, and dried in vacuum at about 55°C for 6 hours to obtain 6.03g of off-white crystalline powder, easily soluble in water, MS (ESI, EI) m / e : 483 (M-18), 351 (M-133); HPLC analysis: the retention time of the main peak of the sample is consistent with the main peak of the lomefloxacin reference substance; melting point: 222.4-225.2°C (ELECTROTHERMAL MELTING POINT APPARATUS, uncorrected), Karl The mois...

Embodiment 2

[0044] Example 2 In a three-necked flask, take 10 g of lomefloxacin hydrochloride and equimolar DL-aspartic acid, dissolve lomefloxacin hydrochloride in water, and adjust the pH value to about 7 with 1M sodium hydroxide solution while stirring , add equimolar DL-aspartic acid, stir to dissolve, let it stand for 1 hour, filter, slowly add 80ml of acetone and 10ml of isopropanol to the filtrate, cool to below 0°C, wait for the solid to precipitate, filter, and use Rinse with acetone for several times, pump dry, recrystallize with appropriate amount of water-acetone, filter under reduced pressure, recrystallize the solid with appropriate amount of water-acetone, filter under reduced pressure, and dry under vacuum at about 40°C for 4 hours to obtain 5.51 g of off-white powder, MS (ESI, EI) m / e: 483 (M-18), 351 (M-133); HPLC analysis: purity 99.5%, the retention time of the main peak of the sample is consistent with that of the lomefloxacin reference substance. Moisture (Karl Fisch...

Embodiment 3

[0047] Example 3 In a three-necked flask, take 10 g of lomefloxacin hydrochloride and equimolar D-aspartic acid, dissolve lomefloxacin hydrochloride in water, and adjust the pH value to 7 with 0.5M sodium hydroxide solution under stirring. Add equimolar D-aspartic acid, stir to dissolve, let it stand for 1 hour, filter, slowly add 100ml of acetone to the filtrate, cool to below 0°C, wait for the solid to precipitate, filter, and rinse the solid with acetone for several Once, drained, water 15ml-acetone 90ml-isopropanol 20ml recrystallized, filtered under reduced pressure, solid water-acetone recrystallized, filtered under reduced pressure, vacuum dried at about 60°C for 4 hours to obtain 5.76g of off-white powder, MS (ESI , EI) m / e: 483 (M-18), 351 (M-133), HPLC analysis: purity 99.6%, the retention time of the main peak of the sample is consistent with that of the lomefloxacin reference substance. Moisture (Karl Fischer method): 2.06%, thermal analysis test (TG-DTA) shows: th...

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PUM

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Abstract

The invention relates to a lomefloxacin aspartate hydrate and its novel preparation method and use. The novel preparation method of the lomefloxacin aspartate hydrate comprises the following steps of dissolving lomefloxacin aspartate in one or more of water, C3-C6 low-grade ketones and C1-C6 low-molecular weight alcohols as solvents in a reactor, adjusting a pH value to 6-8.5 by an alkali, adding L, D or DL aspartic acid or its solution into the reactor, stirring for dissolution so that a reaction is finished, slowly adding one or more of C3-C8 low-grade ketones, C1-C6 low-molecular weight alcohols and C2-C6 low-grade ethers into the reactor, cooling to a temperature of -20 to 20 DEG C, filtering after solids are precipitated, carrying out rinsing by one or more of organic solvents of C1-C6 low-molecular weight alcohols, C3-C8 low-grade ketones, C2-C6 low-grade ethers and C1-C6 low-grade halohydrocarbons, carrying out vacuum-pumping and drying to obtain the lomefloxacin aspartate hydrate. The lomefloxacin aspartate hydrate is powder of which the color changes form almost white to faint yellow and has good storage stability.

Description

technical field [0001] The present invention relates to the technical field of medicine, and specifically provides a new preparation method of lomefloxacin aspartate hydrate, as well as the corresponding crystal hydrate and its application. Background technique [0002] The literature only reported lomefloxacin aspart [C 17 h 19 f 2 N 3 o 3 ·C 4 h 7 NO 4 , Molecular weight: 484.46] and its use as well as the hydrate of lomefloxacin aspartate and its preparation method, but the patent used lomefloxacin base when preparing the hydrate of lomefloxacin aspartate, the starting material The base is difficult to obtain, expensive, and the purification is cumbersome, which is not conducive to the preparation and quality control of the hydrate of lomefloxacin aspartate. Contents of the invention [0003] The present invention relates to a new preparation method of lomefloxacin aspartate hydrate, as well as the corresponding crystalline hydrate and its use. Aspartic acid lo...

Claims

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Application Information

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IPC IPC(8): C07D401/04
Inventor 胡梨芳
Owner 胡梨芳
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