Research speed reading in 2021. In classical electrochemical theory, both the electron transfer rate and the adsorption of reactants at the electrode control the electrochemical reaction. 25537-64-8, name is 4,5-Dibromo-1-methyl-1,2,3-triazole belongs to triazoles compound, it is a common compound, a new synthetic route is introduced below. Recommanded Product: 4,5-Dibromo-1-methyl-1,2,3-triazole
Intermediate 14e (0554) 4,5-Dibromo-2-methyl-2H-l,2,3-triazole Batch 1 : To a solution of 4,5-dibromo-lH-triazole (Intermediate 14f; 490.00 g, 2.16 mol) in DMF (3.2 L) was added potassium carbonate (358.23 g, 2.59 mol). The mixture was cooled to -10C under a nitrogen atmosphere and iodomethane (147.91 mL, 2.38 mol) was added dropwise. The reaction was then stirred at 25C for 16 hours. Batch 2: To a solution of 4,5-dibromo-lH-triazole (Intermediate 14f; 400 g, 1.76 mol, 1.00 eq) in DMF (2.8 L) was added potassium carbonate (291.9 g, 2.11 mol). The mixture was cooled to – 10C under a nitrogen atmosphere and iodomethane (131.48 mL, 2.11 mol) was added dropwise. The reaction was then stirred at 25C for 16 hours. Batches 1 and 2 were then combined and the reaction was quenched by the addition of water (4.2 L) and the aqueous phase extracted with MTBE (7 L x 3). The organic extract was concentrated under vacuum to approximately 700 mL and isopropanol (2 L) was added dropwise. This mixture was then stirred at 25 C for 2 hours and the resulting precipitate filtered and dried under vacuum to afford undesired 4,5-dibromo-l-methyltriazole (220 g, 23.5%) as a solid which showed the following NMR spectral data: FontWeight=”Bold” FontSize=”10″ H NMR (400MHz, CDCb) delta 4.09 (s, 3H). 13CNMR (400MHz, CDCb) delta 123.03, 113.09, 37.00. The filtrate was concentrated under vacuum to afford an oil, isopropanol (1 L) was added and resulting solution was warmed to 50 C and then water (3 L) was added dropwise. The mixture was cooled to 25C and stirred for 5 hours and the resulting precipitate was collected by filtration, washed with water (300 mL x 2) and, dried under vacuum at 50C for 16 hours to afford 4,5-dibromo-2- methyl-2H-l,2,3-triazole (Intermediate 14e; 570 g, 60.8% yield) as a solid. FontWeight=”Bold” FontSize=”10″ H NMR (400MHz, CDCb) delta 4.18 (s, 3H). 13C NMR (400MHz, CDCb) delta 124.25, 43.07.
Balanced chemical reaction does not necessarily reveal either the individual elementary reactions by which a reaction occurs or its rate law. In my other articles, you can also check out more blogs about 25537-64-8, and we look forward to future research findings.
Reference:
Patent; ASTRAZENECA AB; WARD, Richard, Andrew; JONES, Clifford, David; FERON, James, Lyman; (80 pag.)WO2017/80980; (2017); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics