Application of 261762-35-0, These common heterocyclic compound, 261762-35-0, name is 5-Bromo-1,2-difluoro-3-methoxybenzene, 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 50 mL round-bottom flask, introduce 1 g (4.48 mmol) of 5-bromo-2,3-difluoroanisole in 25 mL of dioxane then add 1.708 g (6.73 mmol) of bis(pinacolato)diboron, 1.320 g (13.45 mmol) of potassium acetate and 0.183 g (0.224 mmol) of bis(diphenylphosphino)ferrocene-palladium(II)dichloride dichloromethane complex. The reaction mixture is stirred at 80 C. overnight. After returning to room temperature, the reaction is hydrolyzed by slow addition of water and extracted with ethyl acetate. The organic phase is dried over sodium sulfate, filtered and concentrated. The residue obtained is purified by chromatography on silica gel (eluent: cyclohexane/ethyl acetate: 95:5) to afford 197 mg (15%) of intermediate 13 as a yellow solid. (0484) LCMS (EI, m/z): (M+1) 271.08 (0485) 1H NMR: dH ppm (400 MHz, DMSO): 7.13-7.17 (2H, m, CHarom), 3.90 (3H, m, CH3), 1.30 (12H, m, CH3).
The synthetic route of 261762-35-0 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; PIERRE FABRE MEDICAMENT; KALOUN, El Bachir; GRISONI, Serge; GOMES, Bruno; SCHMITT, Philippe; (43 pag.)US2017/281622; (2017); A1;,
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