Synthetic Route of 7411-23-6, New Advances in Chemical Research in 2021. The appropriate choice of redox mediator can avoid electrode passivation and overpotential, which strongly inhibit the efficient activation of substrates in electrolysis. 7411-23-6, name is 3,5-Dibromo-1H-1,2,4-triazole, molecular formula is C2HBr2N3, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, below Introduce a new synthetic route.
In a 250 mL round bottomed flask, 3,5-dibromo-1H-1,2,4-triazole (Int-1, 2.00 g, 8.82 mmol) was dissolved in DMF (60 mL) and potassium carbonate (2.72 g, 19.5 mmol) was added. After stirring for 20 min at room temperature, 2,2,2-trifluoroethyl trifluoromethanesulfonate (2.32 g, 1.36 mL, 9.70 mmol) was added and the reaction mixture was stirred for 20 h at roomtemperature. After that, it was concentrated in vacuo, combined with ice- water (200 mL) and extracted with MTBE (3 x 200 mL). The combined organic layers were washed with water (2 x 200 mL) and brine (200 mL), dried (sodium sulfate) and concentrated in vacuo to yield the title compound as yellow liquid (2.71 g, 99%) which was used in the next step without further purification. 1H NMR (DMSO-d6, 300 MHz): 5.31 (q, J = 8.8 Hz, 2 H). MS (ES+) m/z 307.9, 309.9, 311.9 [M+H, 2 Br isotopes] .
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Reference:
Patent; F. HOFFMANN-LA ROCHE AG; HOFFMANN-LA ROCHE INC.; BARTELS, Bjoern; BERCHTOLD, Stefan; GALLEY, Guido; GOERGLER, Annick; JAKOB-ROETNE, Roland; KRUMMENACHER, Daniela; LIMBERG, Anja; NEIDHART, Werner; RATNI, Hasane; REUTLINGER, Michael; RODRIGUEZ SARMIENTO, Rosa Maria; SCHNIDER, Christian; (309 pag.)WO2018/87018; (2018); A1;,
1,2,3-Triazole – Wikipedia,
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