New discoveries in chemical research and development in 2021. As an important bridge between the micro and macro material world, chemistry is one of the main methods and means for humans to understand and transform the material world.7343-34-2, name is 3,5-Dimethyl-4H-1,2,4-triazole belongs to triazoles compound, it is a common compound, a new synthetic route is introduced below. Product Details of 7343-34-2
Intermediate 2 4-(3,5-dimethyl-lH-l,2,4-triazol-l-yl)-6-iodo-2-methylpyrimidine (Intermediate 2) A mixture of 4,6-dichloro-2-methylpyrimidine (505 mg, 3.1 mmol), 3,5-dimethyl-lH-l,2,4- triazole (300 mg, 3.1 mmol) and CS2CO3 (1.54 g, 4.7 mmol) in THF (20 mL) was heated at reflux overnight. The mixture was filtered and the filtrate was concentrated to give 4-chloro-6- (3,5-dimethyl-lH-l,2,4-triazol-l-yl)-2-methylpyrimidine that was used without further purification. MS: m/z = 224.1 (M+H). To a mixture of 4-chloro-6-(3,5-dimethyl-lH-l,2,4-triazol-l-yl)-2-methylpyrimidine (2.00 g, 8.9 mmol), KI (4.44 g, 26.8 mmol) was added 57percent aq. HI solution (20 mL, 89.2 mmol). After heating at 70 °C for 5 min, water (20 mL) was added to the reaction mixture. The white solid was filtered, rinsed with water, and dried under vacuum to give Intermediate 2 as a white solid. XH NMR (400 MHz, DMSO) delta 8.06 (s, 1H), 2.78 (s, 3H), 2.62 (s, 3H), 2.30 (s, 3H). MS: m/z = 316.1 (M+H).
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Reference:
Patent; MERCK SHARP & DOHME CORP.; KUDUK, Scott, D.; MCCOMAS, Casey, C.; REGER, Thomas, S.; WO2014/78216; (2014); A1;,
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