Preparation method of moxifloxacin hydrochloride
A technology for moxifloxacin hydrochloride and hydrochloric acid is applied in the field of preparation of moxifloxacin hydrochloride, which can solve the problems of large loss of moxifloxacin hydrochloride, low yield and liquid phase purity, and insufficient product quality, and achieves low total impurity content. , the effect of improving purity and reducing energy consumption
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[0034] Example 1
[0035] A method for preparing moxifloxacin hydrochloride, using ethyl 1-cyclopropyl-6,7-difluoro-1,4-dihydro-8-methoxy-4-oxo-3-quinolinecarboxylate As the parent ring, the condensation is carried out with (S,S)-2,8-diazabicyclo[4,3,0]nonane as the side chain, and after the alkali hydrolysis is completed, 6N hydrochloric acid is added in two portions to continuously crystallize two Secondly, the crystalline product obtained for the second time was recrystallized once with ethanol to obtain moxifloxacin hydrochloride with high content and good quality. Specific steps are as follows:
[0036] (1) Add the weighed boric acid and zinc chloride into the 50L reaction tank, and pump acetic anhydride into the reaction tank. Under stirring, open the jacket for steam heating, heat up to 110℃~120℃, keep the temperature for 2h; end the temperature keeping , Cool down to below 100°C, pump glacial acetic acid into the reaction tank, heat up to 110°C~120°C, keep the temperature...
Example Embodiment
[0049] Example 2
[0050] A method for preparing moxifloxacin hydrochloride, using ethyl 1-cyclopropyl-6,7-difluoro-1,4-dihydro-8-methoxy-4-oxo-3-quinolinecarboxylate As the parent ring, the condensation is carried out with (S,S)-2,8-diazabicyclo[4,3,0]nonane as the side chain, and after the alkali hydrolysis is completed, 6N hydrochloric acid is added in two portions to continuously crystallize two Secondly, the crystalline product obtained for the second time was recrystallized once with ethanol to obtain moxifloxacin hydrochloride with high content and good quality. Specific steps are as follows:
[0051] (1) Add the weighed boric acid and zinc chloride into the 50L reaction tank, and pump acetic anhydride into the reaction tank. Under stirring, open the jacket for steam heating, heat up to 110℃~120℃, keep the temperature for 2h; end the temperature keeping , Cool down to below 100°C, pump glacial acetic acid into the reaction tank, heat up to 110°C~120°C, keep the temperature...
Example Embodiment
[0064] Example 3
[0065] A method for preparing moxifloxacin hydrochloride, using ethyl 1-cyclopropyl-6,7-difluoro-1,4-dihydro-8-methoxy-4-oxo-3-quinolinecarboxylate As the parent ring, the condensation is carried out with (S,S)-2,8-diazabicyclo[4,3,0]nonane as the side chain, and after the alkali hydrolysis is completed, 6N hydrochloric acid is added in two portions to continuously crystallize two Secondly, the crystalline product obtained for the second time was recrystallized once with ethanol to obtain moxifloxacin hydrochloride with high content and good quality. Specific steps are as follows:
[0066] (1) Add the weighed boric acid and zinc chloride into the 50L reaction tank, and pump acetic anhydride into the reaction tank. Under stirring, open the jacket for steam heating, heat up to 110℃~120℃, keep the temperature for 2h; end the temperature keeping , Cool down to below 100°C, pump glacial acetic acid into the reaction tank, heat up to 110°C~120°C, keep the temperature...
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