Synthetic Route of 7343-34-2, New Advances in Chemical Research in 2021.Reactions catalyzed within inorganic and organic materials and at electrochemical interfaces commonly occur at high coverage and in condensed media, 7343-34-2, name is 3,5-Dimethyl-4H-1,2,4-triazole, molecular formula is C4H7N3, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, below Introduce a new synthetic route.
To a slurry of 4,6-dichloro-2-methylpyrirnidine (1-1) (5.00 g, 30.67 mmol, 1.0 eq.) and cesium carbonate (15.0 g, 46.05 mmol, 1.5 eq.) in DMF (250 mL) at 0 °C under nitrogen was added a solution of 3,5-dimethyl-lH-l,2,4-triazole (2.98 g, 30.67 mmol, 1.0 eq.) in DMF (50 mL) via a dropping funnel over 1 hour. The reaction was then warmed to room temperature and stirred for 1 hour. The reaction was quenched by addition of water (500 mL) and extracted with ethyl acetate (3 x 400 mL). The combined organic layers were dried over sodium sulfate, filtered and concentrated to dryness. The crude product was purified by silica gel column chromatography (0-30percent ethyl acetate in hexanes) to afford 4-chloro-6-(3,5-dimethyl-lH-l,2,4-triazol-l-yl)-2-methylpyrimidine (1-2) as a white solid. ‘Eta NMR (300 MHz, CDC13) delta 7.75 (s, 1H), 2.91 (s, 3H), 2.72 (s, 3H), 2.41 (s, 3H). LRMS mlz (M+Ff) 224 found, 224 required.
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Reference:
Patent; MERCK SHARP & DOHME CORP.; COX, Christopher, D.; DUDKIN, Vadim, Y.; KIM, June, J.; KUDUK, Scott, D.; MCVEAN, Carol; REGER, Thomas; STEEN, Justin; STEELE, Thomas; WO2013/52526; (2013); A1;,
1,2,3-Triazole – Wikipedia,
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