These common heterocyclic compound, 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. Product Details of 4923-01-7
A mixture of methyl 3-oxo-2-(4-(4-(trifluoromethoxy)phenyl)piperazin-1 -yl)butanoate (12B) (450 mg, 1 .249 mmol) and 3-methyl-1 H-1 ,2,4-triazol-5-amine (184 mg, 1 .873 mmol) in Acetic Acid (10 mL) was heated at 130 C for 2 h. Then reaction mixtre was diluted with water (25 mL) and adjusted to pH=6 by addition of Na2C03 solution. The resluting mixture was extracted with EtOAc twice. Organic layers were dried over Na2S04 and concentrated to give a crude product that was purified by ISCO with 0-100% EtOAc:EtOH (3:1 ) in hexanes to give two peaks of same mass. Peak two was the desired one based on NMR and LCMS. 1 H NMR (400 MHz, Methanol- d4) delta 7.44 – 7.21 (m, 5H), 5.16 (s, 2H), 4.19 – 3.98 (m, 2H), 3.61 – 3.39 (m, 2H), 3.23 – 2.97 (m, 2H), 2.85 – 2.58 (m, 2H), 2.50 (s, 3H), 2.42 (s, 3H). M/Z (M+H) = 409.1 .
The synthetic route of 5-Methyl-4H-1,2,4-triazol-3-amine has been constantly updated, and we look forward to future research findings.
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,
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