Sitafloxacin hydrate degradation impurity preparation method
A technology for sitafloxacin and impurities, which is applied in the field of preparation of quinolones for degrading impurities of sitafloxacin, achieving the effect of less steps, mild reaction and high commercial value
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Examples
Embodiment 1
[0019] Take 5.0 g of the compound sitafloxacin and add it to 100 ml of purified water as a solvent, and stir to form a suspension. The temperature was controlled at 20°C, and the product was irradiated under a mercury lamp for 10 hours, and the product was obviously formed by TLC detection. The reaction was stopped, and the crude compound was obtained by distillation under reduced pressure, which was separated by column chromatography, and the eluent was dichloromethane:methanol=5:1, and 536mg of the product (P1) and 604mg (P2), respectively, were obtained with a yield of 12.69% and 11.84% respectively. %.
Embodiment 2
[0021] Take 5.0 g of the compound sitafloxacin and add it into the solvent 200 ml of methanol, and stir to form a suspension. The temperature was controlled at 25°C, and the product was irradiated under a mercury lamp for 15 hours, and the product was obviously formed by TLC detection. The reaction was stopped, and the crude compound was obtained by distillation under reduced pressure, which was separated by column chromatography, and the eluent was dichloromethane:methanol=10:1, and the product was 498mg (P1) with a yield of 11.78% and 573mg (P2), with a yield of 11.23 %.
Embodiment 3
[0023] Take 5.0 g of the compound sitafloxacin and add it into 200 ml of acetone as a solvent, and stir to form a suspension. Control the temperature at 25°C and irradiate for 15 hours under an ultraviolet lamp, and TLC detects that a product is obviously formed. The reaction was stopped, and the crude compound was obtained by distillation under reduced pressure. It was separated by column chromatography, and the eluent was dichloromethane:methanol=5:1. The product was 310mg (P1) with a yield of 7.34% and 405mg (P2), with a yield of 7.94% %.
PUM
Abstract
Description
Claims
Application Information
- R&D Engineer
- R&D Manager
- IP Professional
- Industry Leading Data Capabilities
- Powerful AI technology
- Patent DNA Extraction
Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.
© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com