Synthetic Route of 762240-92-6, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 762240-92-6 as follows.
7-[(3R)-3-[N-(tert-butoxycarbonyl)amino]-4-(2,4,5-trifluorophenyl)butanoyl]-3-(trifluoro-methyl)-5,6,7,8-tetrahydro-1,2,4-triazolo[4,3-a]pyrazine (12)To a solution of 3-trifluoromethyl-5,6,7,8-tetrahydro[1,2,4]triazolo[4,3-a]pyrazine hydrochloride (11) (1.0 eq, 28.0 gm), diisopropylethylamine (2.0 eq, 31.0 gm), 1-hydroxybenzotriazole (1.2 eq, 22.0 gm), and EDC-HCl (1.2 eq, 28.0 gm) in N,N-dimethylformamide (4.0 vol, 160.0 ml), a solution of (3R)-3-[N-(tert-butoxycarbonyl)amino]-4-(2,4,5-trifluorophenyl)butanoic acid (07) (40.0 gm, 0.12 mol) in N,N-dimethylformamide (4.0 vol, 160.0 ml) was charged at 0-5 C. within 1 hour. The clear pale yellow solution was further stirred for 12 hours at 25-30 C. After stirring for 12 hours, the N,N-dimethylformamide was distilled out completely at 55-65 C. under reduced pressure to give a brown coloured residue. The brown coloured residue was further basified with 10% Na2CO3 solution (1.0 vol, 40.0 ml) and the product was extracted in ethyl acetate (3×10.0 vol, 3×400.0 ml). The combined ethyl acetate layers were washed with water, charcoalized and filtered, and the ethyl acetate was distilled out completely to give a white coloured product. The product was triturated with hexane (10.0 vol, 400.0 ml) and filtered at 25-30 C. The crude Boc-protected sitagliptin free base (12) was further purified by crystallising it from a mixture of isopropanol (20.0 vol) and water (2.0 vol).Molar Yield: 75-81% (56 gm)Chemical Purity: 95-97% (as measured by HPLC)
According to the analysis of related databases, 762240-92-6, the application of this compound in the production field has become more and more popular.