Electric Literature 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.
3,5-Dibromo-1,2,4-triazole (1; 1.134 g, 5.0 mmol) and 4-chloro-2,6-bis(hydroxymethyl)phenol (2q; 472 mg, 2.5 mmol) were refluxed for5 h in DMF (10 mL). After completion of the reaction, the mixture wascooled and poured into H2O (30 mL). The precipitate formed was collectedby filtration, washed with H2O, dried, and recrystallized; yield:722 mg (55%); colorless crystals; mp 258-260 C (DMF).IR (KBr): 2924, 1601, 1555, 1520, 1470, 1431, 1292, 1261, 1180, 1150,1065, 987, 864 cm-1.1H NMR (400 MHz, DMSO-d6): delta = 7.58 (d, J = 2.3 Hz 1 H, Ar), 7.50 (d,J = 2.3 Hz, 1 H, Ar), 5.47 (s, 2 H, CH2), 5.29 (s, 2 H, CH2).13C NMR (100 MHz, DMSO-d6): delta = 153.2 (C), 145.0 (C), 140.3 (C),137.2 (C), 132.2 (C), 130.6 (CH), 129.2 (C), 128.4 (CH), 124.9 (C), 119.0(C), 48.0 (CH2), 46.1 (CH2).MS for 79Br, 35Cl (EI): m/z (%) = 522 (2, [M]+), 443 (2, [M – Br]+), 364 (1,[M – 2 Br]+), 298 (7, [M – C2Br2N3]+), 218 (5), 177 (5), 156 (21), 153(23, [C8H6ClO]+), 137 (20), 128 (30), 125 (58), 102 (73), 89 (100), 80(65).Anal. Calcd for C12H6Br3ClN6O: C, 27.43; H, 1.15; N, 16.00. Found: C,27.51; H, 1.09; N, 16.09.
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Reference:
Article; Osipov, Dmitry V.; Osyanin, Vitaly A.; Voskressensky, Leonid G.; Klimochkin, Yuri N.; Synthesis; vol. 49; 10; (2017); p. 2286 – 2296;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics