Synthetic Route of 7411-23-6, A common heterocyclic compound, 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, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
A mixture of 3,5-dibromo-1H-1,2,4-triazole (15.5 g, 0.068 mol) andNaHCO3 (6.8 g, 0.082 mol) in DMF (150 mL) was slowly treatedwith 1,2-dibromoethane (26.0 g, 0.137 mol). The mixture was stirredfor overnight at 55 C. Then, the reaction was quenched with water(20 mL) and extracted by EtOAc (60 mL × 2). The organic layer waswashed with brine (40 mL × 2), dried over Na2SO4 and concentrated invacuo. The residue was purified by silica gel column chromatographyto provide compound 20 as: White solid; m.p. 47-48 C; yield 15.5 g(68%); 1H NMR (400 MHz, CDCl3): delta 4.52 (t, J = 6.3 Hz, 2H), 3.72(t, J = 6.3 Hz, 2H); 13C NMR (125 MHz, CDCl3): delta 142.03, 131.66,51.96, 29.10; MS (EI) m/z: 331 (M+). HRMS (EI) m/z calcd forC4H4Br3N3(M+): 330.7955; found: 330.7960.
The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.
Reference:
Article; Zheng, Yazhou; Qian, Anran; Ling, Chenyu; Cao, Xufeng; Cui, Yongmei; Yang, Yushe; Journal of Chemical Research; vol. 41; 4; (2017); p. 241 – 245;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics