Method for preparing ticagrelor solution
A technology of ticagrelor and solution, applied in chemical instruments and methods, blood diseases, pharmaceutical formulations, etc., can solve the problems of reduced yield, increased complexity of preparation process, increased annual production cost and raw material cost, etc.
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Example Embodiment
[0056] Example 1 P = Trityl, P 1 = Hydrogen, P 2 = When hydrogen, the preparation method of ticagrelor solution
[0057] The reaction route is as follows:
[0058]
[0059] The crude ticagrelor was prepared according to the method of Chinese patent CN1200940C, with a purity of 90% (HPLC analysis purity) and a content of 88% (mass fraction).
[0060] Add 88% crude ticagrelor (5.94g, 10.0mmol), triphenylchloromethane (3.62g, 13.0mmol) and dichloromethane (60ml) to a 100ml three-necked round-bottomed flask, and stir. well mixed. The temperature was raised to 25-30°C, triethylamine (1.32g, 13.0mmol) was added dropwise, and the reaction was stirred at this temperature. After reacting for 3 to 4 hours, HPLC tracked the completion of the reaction, and then a saturated ammonium chloride solution (50 ml) was added to quench the reaction. The organic phase was separated, and the aqueous phase was extracted once with dichloromethane (50 ml). The organic phases were combined, washed once wit...
Example Embodiment
[0062] Example 2 P=tert-butyldiphenylsilyl, P 1 = Hydrogen, P 2 = When hydrogen, the preparation method of ticagrelor solution
[0063] The reaction route is as follows:
[0064]
[0065] The crude ticagrelor was prepared according to the method of Chinese patent CN1200940C, with a purity of 90% (HPLC analysis purity) and a content of 88% (mass fraction).
[0066] To a 100ml three-necked round bottom flask was added 88% crude ticagrelor (5.94g, 10.0mmol), tert-butyldiphenylchlorosilane (3.30g, 12.0mmol) and dichloromethane (60ml) , Mix well under stirring. The temperature was raised to 25-30°C, triethylamine (1.21g, 12.0mmol) was added dropwise, and the reaction was stirred at this temperature. After reacting for 2 to 3 hours, HPLC tracked the completion of the reaction, and then a saturated ammonium chloride solution (50 ml) was added to quench the reaction. The organic phase was separated, and the aqueous phase was extracted once with dichloromethane (50 ml). The organic phases...
Example Embodiment
[0068] Example 3 P=4-phenylbenzoyl, P 1 = Hydrogen, P 2 = When hydrogen, the preparation method of ticagrelor solution
[0069] The reaction route is as follows:
[0070]
[0071] The crude ticagrelor was prepared according to the method of Chinese patent CN1200940C, with a purity of 90% (HPLC analysis purity) and a content of 88% (mass fraction).
[0072] Add 88% crude ticagrelor (5.94g, 10.0mmol), triethylamine (1.21g, 12.0mmol), 4-(N,N-dimethylamino) to a 100ml three-necked round bottom flask. Pyridine (0.05g) and dichloromethane (50ml), mix well with stirring. The temperature was raised to 25-30°C, and a dichloromethane solution of 4-phenylbenzoyl chloride (2.60 g, 12.0 mmol) was added dropwise, and the reaction was stirred at this temperature. After 4 hours of reaction, after HPLC tracked the completion of the reaction, saturated ammonium chloride solution (50ml) was added to quench the reaction. The organic phase was separated, and the aqueous phase was extracted once with d...
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