Reference of 4923-01-7, New discoveries in chemical research and development in 2021. We’ll be discussing some of the latest developments in chemical about CAS: 4923-01-7, name is 5-Methyl-4H-1,2,4-triazol-3-amine, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
A mixture of methyl 3-oxo-2-(4-phenethylpiperidin-1 -yl)butanoate (1 A) (11 g, 36.3 mmol), 3- methyl-1 H-1 ,2,4-triazol-5-amine (8.89 g, 91 mmol) and 4-methylbenzenesulfonic acid (6.24g, (0229) 36.3 mmol) was heated from 140C to 160 C with vigorous stirring using a stir bar. The reaction mixture changed from solid to liquid, which then turned into a solid again. The crude mixture was dissolved in MeOH (150 ml_) and divided into three portions. Each portion was purified using a 330 grams combiflash column eluting with 0.1 to 3% MeOH in DCM to give (1 ). 1 H NMR (400 MHz, DMSO-d6) delta 12.83 (s, 1 H), 7.32 – 7.25 (m, 2H), 7.24 – 7.20 (m, 2H), 7.20 – 7.13 (m, 1 H), 3.40 (t, J = 10.4 Hz, 2H), 2.68 – 2.56 (m, 4H), 2.22 (s, 3H), 2.19 (s, 3H), 1 .75 – 1 .64 (m, 2H), 1 .61 – 1 .46 (m, 2H), 1 .30 – 1 .13 (m, 3H). Method 2: RT = 3.37 min.; M/Z (M+H) = 352.3.
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Reference:
Patent; NOVARTIS AG; CHIANELLI, Donatella; GIBNEY, Michael; LERARIO, Isabelle K.; LIANG, Fang; LIU, Xiaodong; MOLTENI, Valentina; NAGLE, Advait Suresh; SMITH, Jeffrey M.; SUPEK, Frantisek; XIE, Yongping; YEH, Vince; (64 pag.)WO2018/229683; (2018); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics