Electric Literature of 7170-01-6, A common heterocyclic compound, 7170-01-6, name is 3-Methyl-1H-1,2,4-triazole, molecular formula is C3H5N3, 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.
To a mixture of the intermediate 5 500 mg, 60% sodium hydride (dispersion in paraffin liquid) 60 mg and N,N-dimethylformamide 2.5 mL was added 3-methyl-1H-1,2,4-triazole (which was prepared by a method described in US 2006/0293304 A1) 113 mg. The mixtures were stirred at 0C for 2.5 hours. To the reaction mixture was then added saturated aqueous sodium hydrogen carbonate solution and the mixtures were extracted with ethyl acetate. The organic layers were washed with water and brine and dried over anhydrous sodium sulfate. The resulting organic layers were concentrated under reduced pressure. The resulting residues were subjected to a silica gel colunm chromatography to give the present compound 4 153 mg. H1-NMR (CDCl3) delta: 9.03 (1H, s), 8.80 (1H, br s), 8.68 (1H, d), 8.35 (1H, br s), 8.22 (1H, d), 3.92 (3H, s), 3.81 (2H, q), 2.54 (3H, s), 1.39 (3H, t).
The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.
Reference:
Patent; Sumitomo Chemical Company, Limited; TANABE, Takamasa; MIZUNO, Hajime; OKAMOTO, Hiroshi; (41 pag.)US2017/135348; (2017); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics