Continuously updated synthesis method about 767340-03-4

Adding a certain compound to certain chemical reactions, such as: 767340-03-4, name is (2Z)-4-Oxo-4-[3-(trifluoromethyl)-5,6-dihydro[1,2,4]triazolo[4,3-a]pyrazine-7(8H)-yl]-1-(2,4,5-trifluorophenyl)but-2-en-2-amine, belongs to Pyrazines compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 767340-03-4, SDS of cas: 767340-03-4

To degaussed 2,2,2-trifluoroethanol (TFE) (30 mL) were added Rhodium(I) chloride 1,5- cycloocatadiene complex (18.3 mg, 0.05percent) and (R)-(-)-l-[(S)-2- diphenylphosphino)ferrocenyl]ethyl di-tert-butylphosphine (44.2 mg, 0.11percent). The solution was stirred at room temperature, degaussed three times, and then stirred for one hour at room temperature.To 250 ml hydrogenator were added (Z)-3-amino-l-(3-(trifluoromethyl)-5,6-dihydro- [l,2,4]triazolo[4,3-a]pyrazyn-7(8H)-yl)-4-(2,4,5-trifluorophenyl)but-2-en-l-one (30 gr, 1 equivalent) and TFE (120 ml) at room temperature and the mixture was washed three times with nitrogen gas. The catalyst solution was added and the clear solution was washed three times with nitrogen gas and then with hydrogen gas. The mixture remained under hydrogen at constant pressure of 5 bar and heated to 550C. The mixture was stirred at 550C for 26 hours to obtain Sitagliptin base in TFE solution (optical purity by HPLC 76.9percent, purity by HPLC 91.5percent)Two reaction mixtures which were obtained according to the above procedure were combined and the solution was divided to 10 parts.7 parts of the solution, each contained ca~ 6 gr Sitagliptin were concentrated and Sitagliptin base was precipitated by addition of MTBE then filtrated by vacuum filtration. The combined mother liqueur from the crystallization experiments was concentrated. The residue was dissolved in isopropanol (40 mL) at room temperature, heated to 50¡ãC. A solution of phosphoric acid (85percent, 1.7 mL, ca ~1 eq) in isopropanol (20 mL) was added and the mixture kept stirring at 50¡ãC for one hour, then cooled gradually to 25 ¡ãC, and stirred at 25¡ãC over night.The product was isolated by vacuum filtration and dried at 40¡ãC vacuum oven over night to obtain Sitagliptin phosphate crystalline form VI (optical purity by HPLC 51.8percent, purity by HPLC 99.20percent).

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Reference:
Patent; TEVA PHARMACEUTICAL INDUSTRIES LTD.; TEVA PHARMACEUTICALS USA, INC.; WO2009/120746; (2009); A2;,
Pyrazine – Wikipedia,
Pyrazine | C4H4N2 – PubChem