Preparation method of cefcapene diisopropylamine salt
A technology of diisopropylamine salt and cefcapine, which is applied in the field of cephalosporin antibiotics, can solve the problems of unfavorable industrial production, high cost, and difficulty in conforming to pharmaceutical intermediates, and achieves the effects of being convenient for large-scale production and easy to operate.
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Examples
Embodiment 1
[0022] Take 29.8g (0.10mol) of raw material 1 in a reaction flask, add 250ml of dichloromethane and 10.1g (0.10mol) of triethylamine to dissolve, cool to -10°C, slowly add 13.1g (0.11mol) of thionyl chloride dropwise Reagents, after stirring for 1 hour at this temperature. Slowly add 26.7g (0.10mol) of hydrochloride of 7-HACA, 20ml of methanol and 22.8ml (20.2g, 0.2mol) of triethylamine and 1.22g (0.01mol) of 4-dimethylamino in the solution after the reaction For a solution composed of pyridine, keep the reaction solution at -10°C and continue stirring for 2 hours, filter, collect the filtrate, and adjust the pH of the filtrate to 8 with 5% sodium hydroxide solution. The aqueous layer was separated, decolorized, and then 1mol / L hydrochloric acid was added dropwise to pH=2, filtered, washed, and vacuum-dried to obtain 47.1g of intermediate product 5 with a yield of 92.1% and a content of 95.2% by HPLC normalization method.
[0023] Dissolve 25.5g (0.05mol) of the obtained inte...
Embodiment 2
[0025] Take 298g (1.0mol) of raw material 1 in a reaction flask, add 2500ml of dichloromethane and 101g (1.0mol) of triethylamine to dissolve, cool to -10°C, slowly add 131g (1.1mol) of thionyl chloride reagent dropwise, in After stirring at this temperature for 1 hour. Slowly add 267g (1.0mol) of 7-HACA hydrochloride, 200ml of methanol, 228ml (202g, 2.0mol) of triethylamine and 12.2g (0.1mol) of 4-dimethylaminopyridine to the reacted solution solution, keep the reaction solution at -10°C and continue to stir for 3 hours, filter, collect the filtrate, and adjust the pH of the filtrate to 8 with 5% sodium hydroxide solution. The aqueous layer was separated, decolorized, and then 1mol / L hydrochloric acid was added dropwise to pH=2, filtered, washed, and vacuum-dried to obtain 462g of intermediate product 5, with a yield of 90.6% and a content of 94.7% by HPLC normalization method.
[0026] Dissolve 255g (0.5mol) of the obtained intermediate product 5 in 2000ml of dichloromethan...
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