- Refining method of ciprofloxacin and meglumine hydrochloride thereof
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The invention provides a preparation process of ciprofloxacin and meglumine thereof. The intermediate product DLSX07 is stirred at Branson ° C. 20% minutes and then sonicated until the solution is cloudy, stirred at room temperature for a period 30s, stirred at room temperature 3h, cooled and slowly added to distilled water, and filtered through suction filtration and filter cake vacuum drying to obtain a pale yellow powder, and 4% the KOH mixture is subjected to ultrasonic treatment 40 - 50 °C. 1. The process is performed by stirring 5h. NCS .t. The solution is cloudy. LC-MS / MS detection powder is deltafloxacin, distilled water is added, and meglumine is mixed to obtain a deltafloxacin meglumine salt. By optimizing the preparation process, the use of the organic solvent is reduced, the reaction time is shortened, and the ice bath and the addition of the interface carrier material contribute to the improvement of the yield.
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- Preparation method of Delafloxacin and intermediates thereof
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The invention relates to a preparation method of Delafloxacin and intermediates thereof. The method comprises the following steps: firstly, taking 3-chloro-2,4,5-fluorobenzoic acid (compound 1) as a raw material and reacting the raw material with thionyl
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- Preparation of deller floxacin and intermediate thereof
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The invention relates to preparation of deller floxacin and an intermediate thereof. According to the preparation method of the deller floxacin, the purity of an intermediate compound, a compound A-3and a compound W-4 is limited to be more than 99.0 perce
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Paragraph 0075; 0077
(2018/05/30)
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- Preparation method of high-purity delafloxacin meglumine salt
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The invention relates to a method for refining a delafloxacin intermediate compound shown in a formula I. The method comprises the following steps: dissolving the compound in the formula I in a good solvent, mixing the compound with a poor solvent, heatin
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- A method for preparing high-purity delafloxacin
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The invention belongs to the technical field of a high purity delafloxacin preparation method. The high purity delafloxacin preparation method is as follows: a compound shown as formula 14 is hydrolyzed into a salt, a purified solid salt is obtained by solid-liquid separation, and then the purified solid salt is acidified to obtain delafloxacin. The delafloxacin prepared by synthesis methods in the prior art is low in purity, and needs to be further refined; according to the high purity delafloxacin preparation method, a delafloxacin ester derivative is hydrolyzed into a salt, after separation, the salt is acidified for effective removal of impurities, so that the product delafloxacin can reach a high purity (more than 99.5%), and can meet the subsequent preparation requirements; by the high purity delafloxacin preparation method, the objective of refinement can be achieved in the reaction route, a further purification process is omitted, and the operation efficiency and the total yield are improved.
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- PROCESS FOR MAKING QUINOLONE COMPOUNDS
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The present invention relates to the field of synthesizing anti-infective compounds. More particularly, the invention relates to synthesizing a family of quinolone compounds useful as anti-infective agents. The invention includes a process for preparing a
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Page/Page column 14-15; 20-21
(2010/04/27)
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- Identification and suppression of a dimer impurity in the development of delafloxacin
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Delafloxacin is a 6-fluoroquinolone antibiotic which is under development at Rib-X Pharmaceuticals. During initial scale-up runs to prepare delafloxacin, up to 0.43% of a new impurity arose in the penultimate chlorination step. This was identified as a di
- Hanselmann, Roger,Johnson, Graham,Reeve, Maxwell M.,Huang, Shu-Ting
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experimental part
p. 54 - 59
(2010/04/22)
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- Chlorination at the 8-position of a functionalized quinolone and the synthesis of quinolone antibiotic ABT-492
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The total synthesis of quinolone antibiotic ABT-492 has been achieved in 67% yield over nine steps from 2,4,5-trifluorobenzoic acid. The highlights of this synthesis include a novel chemoselective chlorination at the 8-position of a highly elaborated quinolone core. In addition, a Lewis acid promoted cyclization reaction to form the quinolone heterocycle was developed which was incorporated into a one-pot, three-step cyclization/coupling/protection sequence that proceeds in 93% yield.
- Barnes, David M.,Christesen, Alan C.,Engstrom, Kenneth M.,Haight, Anthony R.,Hsu, Margaret C.,Lee, Elaine C.,Peterson, Matthew J.,Plata, Daniel J.,Raje, Prasad S.,Stoner, Eric J.,Tedrow, Jason S.,Wagaw, Seble
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p. 803 - 807
(2012/12/22)
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- PREPARATION OF PYRIDONECARBOXYLIC ACID ANTIBACTERIALS
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A process for making 1-(6-amino-3,5-difluoropyridin-2-yl)-8-chloro-6-fluoro-7-(3-hydroxyazetidin-1-yl)-4-oxo-1,4-dihydro-3-quinolinecarboxylic acid, and therapeutically acceptable salts thereof, and intermediates used in the process are disclosed.
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Page/Page column 17
(2008/06/13)
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- Pyridonecarboxylic acid derivatives or their salts and antibacterial agent comprising the same as the active ingredient
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A pyridonecarboxylic acid derivative represented by the following general formula (1): STR1 [wherein R1 represents hydrogen atom or a carboxyl protective group; R2 represents hydroxyl group, a lower alkoxy group, or a substituted or unsubstituted amino group; R3 represents hydrogen atom or a halogen atom; R4 represents hydrogen atom or a halogen atom; R5 represents a halogen atom or an optionally substituted saturated cyclic amino group; R6 represents hydrogen atom, a halogen atom, nitro group, or an optionally protected amino group; X, Y and Z may be the same or different and respectively represent nitrogen atom, --CH= or --CR7 = (wherein R7 represents a lower alkyl group, a halogen atom, or cyano group) (with the proviso that at least one of X, Y and Z represent the nitrogen atom), and W represents nitrogen atom or --CR8 = (wherein R8 represents hydrogen atom, a halogen atom, or a lower alkyl group)] or its salt, as well as an antibacterial agent containing such compound are provided.
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