Extracurricular laboratory: Synthetic route of 7411-23-6

I hope this article can help some friends in scientific research. I am very proud of our efforts over the past few months and hope to 3,5-Dibromo-1H-1,2,4-triazole help many people in the next few years.

New discoveries in chemical research and development in 2021. The transformation of simple hydrocarbons into more complex and valuable products via catalytic C–H bond functionalisation has revolutionised modern synthetic chemistry. 7411-23-6, name is 3,5-Dibromo-1H-1,2,4-triazole belongs to triazoles compound, it is a common compound, a new synthetic route is introduced below. Safety of 3,5-Dibromo-1H-1,2,4-triazole

An argon gas atmosphere was prepared in a reaction vessel, then, a compound MC7-a (100 g), potassium carbonate (110 g) and N,N?-dimethylformamide (500 mL) were added, and the mixture was heated up to 90 C. Thereafter, to this was added an N,N?-dimethylformamide (100 mL) solution containing a compound MC7-b (109 g), and the mixture was stirred at 100 C. for 1 hour. Thereafter, the mixture was cooled down to room temperature, ion exchanged water and chloroform were added, and the organic layer was extracted. The resultant organic layer was washed with ion exchanged water, dried over anhydrous magnesium sulfate, then, filtered through a filter paved with silica gel, and the resultant filtrate was concentrated under reduced pressure, thereby obtaining an oil. The resultant oil was purified by silica gel column chromatography (a mixed solvent of heptane and ethyl acetate), then, dried under reduced pressure at 45 C., thereby obtaining a compound MC7-c (117 g, yield: 94%) as a colorless oil. The compound MC7-c showed a HPLC area percentage value of 99.5% or more. This operation was conducted repeatedly, thereby obtaining a necessary amount of the compound MC7-c. (0446) TLC/MS (DART, positive): m/z=281.9 [M+H]+ (0447) 1H-NMR (CD2Cl2, 300 MHz): delta (ppm)=3.94 (d, 2H), 2.32-2.23 (m, 1H), 0.95 (d, 6H).

I hope this article can help some friends in scientific research. I am very proud of our efforts over the past few months and hope to 3,5-Dibromo-1H-1,2,4-triazole help many people in the next few years.

Reference:
Patent; Sumitomo Chemical Company, Limited; ABE, Taichi; ASADA, Kohei; OHUCHI, Kazuei; (80 pag.)US2017/166599; (2017); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics