Method for purifying compound
A compound and mixed solution technology, applied in the direction of organic chemistry, can solve the problems of reducing equipment production efficiency, safety hazards, and increasing production costs, and achieve the effects of easy control, improved production efficiency, and less by-products
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Example Embodiment
[0068] Example 1
[0069] Take a 250ml single-mouth bottle, add 10g crude apixaban (purity 95.4%) and 80ml ethylene glycol solution containing 10% ammonia, heat to 90℃ to dissolve, then add 80ml water to cool 40~50℃ and stir for 2 hours , Cool down to 0~10℃. Then it was filtered and dried to obtain 8.9 g of off-white solid with a yield of 89% and a purity of 99.97% by HPLC.
[0070] Spectral data:
[0071] EI-MS(m / z): 460.2;
[0072] 1 H-NMR (500MHz, CDCl 3 , Ppm), δ: 7.49 (d, J = 8.8 Hz, 2H), 7.36 (d, J = 8.8 Hz, 2H), 7.27 (d, J = 8.8 Hz, 2H), 6.95 (d, J = 8.8 Hz , 2H), 6.88 (br, 1H), 5.59 (br, 2H), 4.13 (t, J = 6.6 Hz, 2H), 3.84 (s, 3H), 3.61 to 3.60 (m, 2H), 3.39 (t, J=6.8 Hz, 2H), 2.57 (t, J=5.6 Hz, 2H), 1.94 to 1.96 (m, 4H).
Example Embodiment
[0073] Example 2
[0074] Take a 250ml single-necked bottle, add 10g crude apixaban (purity 95.4%) and 160ml 5% triethylamine in ethylene glycol solution, heat it until it is clear, then add 100ml water to cool down at 40~50℃ and stir 2 Hours, cooling down to 0~10℃. Then, it was filtered and dried to obtain 8.5 g of off-white solid with a yield of 85% and an HPLC purity of 99.96%.
Example Embodiment
[0075] Example 3
[0076] Take a 250ml single-necked flask, add 10g crude apixaban (purity 95.4%) and 100ml methanol solution containing 20% ammonia, heat to clear, then add 40ml water to cool down and stir for 2 hours at 40~50℃, and cool to 0~10℃. Then, it was filtered and dried to obtain 8.6 g of off-white solid with a yield of 86% and an HPLC purity of 99.95%.
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.
© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap