Method for synthesizing 2,2'-biquinoline
A synthetic method, the technology of biquinoline, applied in 2 fields, can solve the problems of unfavorable industrial production, expensive catalysts, high cost of raw materials, etc., and achieve the effects of low cost, no reduction in yield, high product yield and purity
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0026] In a 50 mL round-bottomed flask, H was added sequentially 2 O (5.0g), PEG-400 (1.0g), quinoline (1.0g), after stirring evenly, 1% Pd / C catalyst (0.1g) was added to react at 80°C for 20h, the reaction solution was cooled and suction filtered, The filter cake Pd / C is washed with water, and can be recovered and reused; the filtrate is extracted with ethyl acetate, the solvent is evaporated, concentrated, and crystals are separated out to obtain a crude product, which is recrystallized to obtain 0.12 g of white 2,2'-biquinoline crystals, The yield is 11.9%, and the melting point is 196-197°C. 1 H NMR (400MHz, CDCl 3 ) δppm: 8.86 (d, 2H, J=8.1Hz), 8.34 (d, 2H, J=8.6Hz), 8.25 (dd, 2H, J=2.4Hz), 7.89 (dd, 2H, J=7.0Hz) , 7.59 (m, 2H), 7.77 (m, 2H); 13 C NMR (CDCl 3 ) δppm: 152, 147.5, 137, 129.5, 128.0, 127.5, 127.0, 119.0; MS (EI): m / z (%): 256 (100) [M + ], 128(30), 101(13).
Embodiment 2
[0028] In a 50 mL round-bottomed flask, H was added sequentially 2 O (1.0g), PEG-1000 (2.0g), quinoline (1.0g), after stirring evenly, 10% Pd / C catalyst (0.4g) was added to react at 140°C for 15h, the reaction solution was cooled and suction filtered, The filter cake Pd / C is washed with water and can be recovered and reused; the filtrate is extracted with ethyl acetate, the solvent is evaporated, concentrated, and crystals are precipitated to obtain a crude product, which is recrystallized to obtain 0.53 g of white crystals, the yield is 52.6%.
Embodiment 3
[0030] In a 50 mL round-bottomed flask, H was added sequentially 2 O (3.0g), PEG-400 (3.0g), quinoline (1.0g), after stirring evenly, 5% Pd / C catalyst (1.0g) was added to react at 120°C for 4h, the reaction solution was cooled and suction filtered, The filter cake Pd / C is washed with water and can be recovered and reused; the filtrate is extracted with ethyl acetate, the solvent is evaporated, concentrated, and crystals are precipitated to obtain a crude product, which is recrystallized to obtain 0.58 g of white crystals, the yield is 57.6%.
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