Synthetic Route of 288-88-0, New Advances in Chemical Research in 2021.In classical electrochemical theory, both the electron transfer rate and the adsorption of reactants at the electrode control the electrochemical reaction. 288-88-0, name is 1H-1,2,4-Triazole, molecular formula is C2H3N3, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, below Introduce a new synthetic route.
14a p-(1,2,4-Triazol-1-yl)benzaldehyde and p-(1,2,4-Triazol-4-yl)benzaldehyde 21 ml (200 mmol) of 4-fluorobenzaldehyde (Fluka, Buchs, Switzerland), 30.48 g (220 mmol) of potassium carbonate and 13.8 g (200 mmol) of 1,2,4-triazole (Fluka, Buchs, Switzerland) are suspended in 100 ml of pyridine, after which 1.2 g of copper(I) oxide are added. The reaction mixture is boiled at reflux for 16 h. After that, the solvent is removed and the residue is taken up twice in toluene, followed by evaporation, and dissolved in methylene chloride. The insoluble material is removed by filtration and the solution is concentrated. This yields a mixture of the two 1,2,4-triazol-1-yl- and 1,2,4-triazol-4-yl-substituted benzaldehyde, which can be separated, after digesting with hexane, by means of chromatography on silica gel (mobile solvent: hexane/ethyl acetate 1:1, ethyl acetate and methylene chloride/5% methanol). p-(1,2,4-Triazol-1-yl)benzaldehyde: HPLC20-100: tret=8.50. 1H NMR (DMSO-D6; 200 MHz): 10.04/s (1H); 9.47/s (1H); 8.31/s (1H); 8.12 and 8.09/in each case d, J=10 (2*2H). p-(1,2,4-Triazol-4-yl)benzaldehyde: HPLC20-100: tret=5.96. 1H NMR (DMSO-D6; 200 MHz): 10.05/s (1H); 9.27/s (1H); 8.31/s (1H); 8.09 and 7.98/in each case d, J=9 (2*2H).
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Reference:
Patent; Novatis AG; US6451973; (2002); B1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics