Electric Literature of 7411-23-6, These common heterocyclic compound, 7411-23-6, name is 3,5-Dibromo-1H-1,2,4-triazole, 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.
In a 250 mL round bottomed flask, 3,5-dibromo-1H-1,2,4-triazole (Int-1, 8.00 g, 35.3 mmol) was dissolved in DMF (80 mL) and the solution was cooled to 0-5 C (ice bath). Sodium hydride (60% dispersion in mineral oil, 1.69 g, 42.3 mmol) was added in portions and the resulting mixture was stirred for 45 min at 0-5 C and for 15 min at room temperature. After that, iodomethane (10.0 g, 4.41 mL, 70.5 mmol) was added dropwise at 0-5 C (ice bath). The resulting mixture was stirred for 18 h at room temperature. After that, it was concentrated in vacuo, the residue was diluted with ethyl acetate (200 mL) and water (200 mL), the aqueous phase was extracted with ethyl acetate (2 x 200 mL). The combined organic layers were dried (sodium sulfate) and concentrated in vacuo to yield the title compound as light yellow solid (8.15 g, 96%). 1H NMR (CDCl3, 300 MHz): delta 3.89 (3 H). MS (ES+) m/z 240.0, 242.0, 244.0 [M+H, 2 Br isotopes].
Statistics shows that 3,5-Dibromo-1H-1,2,4-triazole is playing an increasingly important role. we look forward to future research findings about 7411-23-6.
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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