Synthetic method for drug intermediate diphenylethanedione
A technology of diphenylethanedione and a synthesis method is applied in the synthesis of pharmaceutical intermediate diphenylethylenedione, and the field of preparation of pharmaceutical intermediates, and can solve the health damage of reaction operators, high pollution treatment cost, and reaction process. Intense and other problems, to achieve the effect of reducing the risk factor of the reaction, reducing the production cost, and improving the reaction yield
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Example Embodiment
[0018] Example 1:
[0019] The method for synthesizing drug intermediate diphenyl ethylenedione includes the following steps:
[0020] A: Add 2mol 2-bromo-2'-hydroxy-diphenyl-2-methylethanone into the reaction vessel, raise the temperature to 50℃, and then add 900ml of potassium chloride solution with a mass fraction of 9% to react 2h, gradually increase the temperature, and increase the temperature to 70℃ within 60min;
[0021] B: Control the stirring speed to 150rpm, add 4mol of 30% isoamyl butyrate solution, add diocene dimethyl titanium in 5 times within 60min, continue the reaction for 2h, then add 1.2L with a mass fraction of 10% Sodium sulfate solution, stir for 90min, add 15% potassium carbonate solution to adjust the pH to 10, lower the temperature to 10℃, add 800ml 20% sodium chloride solution, precipitate solid, filter, the mass fraction is Wash 4 times with 40% didecylamine solution, wash 2 times with 60% p-cresol solution, recrystallize in 80% 3-dimethylaminopropionitr...
Example Embodiment
[0022] Example 2:
[0023] The method for synthesizing drug intermediate diphenyl ethylenedione includes the following steps:
[0024] A: Add 2mol 2-bromo-2'-hydroxy-diphenyl-2-methylethanone into the reaction vessel, raise the temperature to 58℃, and then add 900ml of potassium chloride solution with a mass fraction of 12% to react 2.1h, gradually increase the temperature, and increase the temperature to 75℃ within 65min;
[0025] B: Control the stirring speed to 180rpm, add 5mol of 32% isoamyl butyrate solution, add diocene dimethyl titanium in 6 times within 87min, continue the reaction for 2.2h, then add 1.2L with a mass fraction of 16 % Sodium sulfate solution, stir for 100min, add 17% potassium carbonate solution to adjust the pH to 10.5, lower the temperature to 12℃, add 800ml 22% sodium chloride solution, precipitate solids, filter, mass fraction Wash 5 times with 42% didecylamine solution, wash 3 times with 62% p-cresol solution, recrystallize in 83% 3-dimethylaminopropion...
Example Embodiment
[0026] Example 3:
[0027] The method for synthesizing drug intermediate diphenyl ethylenedione includes the following steps:
[0028] A: Add 2mol 2-bromo-2'-hydroxy-diphenyl-2-methylethanone into the reaction vessel, raise the temperature to 60℃, and then add 900ml of potassium chloride solution with a mass fraction of 15% to react 3h, gradually increase the temperature, and increase the temperature to 76℃ within 80min;
[0029] B: Control the stirring speed at 190rpm, add 6mol of 36% isoamyl butyrate solution, add diocene dimethyl titanium in 7 times within 90min, continue the reaction for 3h, then add 1.2L with a mass fraction of 17% Sodium sulfate solution, stir for 110min, add 22% potassium carbonate solution to adjust the pH to 11, reduce the temperature to 16℃, add 800ml of 26% sodium chloride solution, precipitate solids, filter, mass fraction Wash 6 times with 45% didecylamine solution, wash 4 times with 66% p-cresol solution, recrystallize in 87% 3-dimethylaminopropionitr...
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.
© 2023 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap