In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 7411-23-6 as follows. Quality Control of 3,5-Dibromo-1H-1,2,4-triazole
To a solution of 3,5-dibromo-1H-1,2,4-triazole (Int-1, 5.0 g, 22.0 mmol) in DMF (70 mL) was added sodium hydride (793 mg, 33.1 mmol) at 0C under argon atmosphere. After complete addition reaction was allowed to stir at 25C for 30 min. Then 2-iodopropane (2.6 mL, 26.4 mmol) was added followed by stirring at 40C for 4 h. After complete consumption of starting material (as monitored by TLC) reaction mixture was poured into ice-water followed by extraction with MTBE. The organic layer was separated and dried over sodium sulphate. Solvent was evaporated under reduced pressure to afford the title compound as yellow liquid (5.4 g, crude) which was sufficiently pure for use in next step. 1H NMR (DMSO-d6, 400 MHz): 1.39 (d, J = 6.6 Hz, 6 H), 4.64-4.71 (m, 1 H). MS (ES+) m/z 270.0 [M+H].
According to the analysis of related databases, 7411-23-6, the application of this compound in the production field has become more and more popular.
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;,
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