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Method for preparing decarboxylated levofloxacin

A technology for decarboxylated levofloxacin and levofloxacin is applied in the field of preparation of decarboxylated levofloxacin to achieve the effects of high yield, improved conversion rate and easy preparation

Active Publication Date: 2012-11-14
YABAO PHARMA GRP CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the structural research of this impurity has been reported in literature abroad, there is no public report on its preparation method at home and abroad.

Method used

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  • Method for preparing decarboxylated levofloxacin
  • Method for preparing decarboxylated levofloxacin

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Embodiment Construction

[0026] The method of the present invention will be further described below in combination with specific embodiments.

[0027] Take 0.03 mol of levofloxacin with a mass of 10.83 g, put it into a pressure-resistant reaction bottle equipped with a spherical condenser, add 1000 ml of 1 mol / L hydrochloric acid solution, stir and dissolve at 60-80°C, and dissolve at 120°C and 0.3Mpa Heat for 50 hours, evaporate the solution to dryness in a water bath at 100°C, and at the same time completely volatilize HCL to obtain a residue of 9.45 g; take the residue and perform repeated recrystallization with a mixed solvent with a volume ratio of ethanol:acetone of 2:1, and the recrystallization includes the following steps :

[0028] (1) Crystallization: add 100 times the weight of the residue to a mixed solvent, heat to 80°C, stir to dissolve the residue, filter, concentrate the filtrate to 2 / 3, put it in a refrigerator at 4°C for 2 hours, precipitate crystals, filter, and use for crystals W...

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Abstract

The invention relates to a method for preparing decarboxylated levofloxacin, which belongs to the technical field of medicinal levofloxacin. The method comprises: mixing levofloxacin and hydrochloric acid at a concentration of 1mol / L according to a ratio of 0.03mol:1,000ml, stirring at 60 to 80 DEG C for dissolution, reacting at 120 DEG C and under a condition of 0.3Mpa for 50 hours to obtain reaction solution, evaporating reaction solution till dryness, recrystallizing residue by using mixed solvent of ethanol and acetone in a volume ratio of 2:1 as a recrystallizing solvent and thus, obtaining the decarboxylated levofloxacin. The selection of a reagent is convenient for subsequent separation operation, and specific reaction temperature, pressure and time are set to improve the conversation rate of the levofloxacin and reduce the generation of impurities. The method has fewer steps, high yield and easy preparation process, and can greatly lower the cost of a decarboxylated levofloxacin reference; and through the recrystallization by using the mixed solvent in a molar ratio of 2:1, the purity of decarboxylated levofloxacin reaches 99.5 percent, and the decarboxylated levofloxacin can be used as a working reference.

Description

technical field [0001] The invention relates to the technical field of medicine levofloxacin, in particular to a preparation method of decarboxylevofloxacin. Background technique [0002] Levofloxacin is the left-handed form of ofloxacin, which has the characteristics of broad antibacterial spectrum and strong antibacterial effect. Japan's Daiichi Pharmaceutical Co., Ltd. launched levofloxacin raw materials and tablets in Japan in 1993, and is now on the market in the United Kingdom, the United States and other countries. Levofloxacin preparations currently on the market in China mainly include tablets, small needles, glucose injections and eye drops. At present, many documents at home and abroad have reported the known impurities of ofloxacin, but there are few research reports on the known impurities of levofloxacin. However, it can be inferred from the known impurities of ofloxacin and the synthesis route that levofloxacin probably contains the same For process impuri...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D498/06
Inventor 王维剑李军谢元超刘琦张中湖
Owner YABAO PHARMA GRP CO LTD