Electric Literature of 399-94-0,Some common heterocyclic compound, 399-94-0, name is 1-Bromo-2,5-difluorobenzene, molecular formula is C6H3BrF2, 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.
Under the protection of nitrogen, 2,5-difluorobromobenzene (15.05g, 78mmol) is dissolved in dry toluene (50 ml), lowering the temperature to ice salt bath -10 C following, dropwise adding isopropyl magnesium chloride/tetrahydrofuran solution of lithium chloride (66 ml, 1.3 mol/L), maintained at about -10 C stirring 1 hour. the1D (10g, 39mmol) dissolved in dry tetrahydrofuran (100 ml) in, is dropped is added to the reaction solution, maintaining the temperature -10 C, canada finishes, to react at room temperature for 4 hours. The temperature dropped to about -10 C, dropwise adding saturated ammonium chloride solution (40 ml), stirring 10 minutes, for 3 mol/L hydrochloric acid solution to adjust pH value to 5 – 6, layered, 3rd phase for methyl tert-butyl ether (50mL × 2) extraction, the combined organic phase, saturated sodium chloride solution (30mL × 2) washing, drying of the organic phase by adding anhydrous sodium sulfate, filtered, concentrated, column chromatography (petroleum ether/ethyl acetate=50:1 – 8:1 (v/v)), get the yellow solid1E(10.1g, 83.5% yield).
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-Bromo-2,5-difluorobenzene, its application will become more common.
Reference:
Patent; SICHUAN HAISCO PHARMACEUTICAL CO., LTD; ZHANG, CHEN; FAN, JIANG; LI, CAI-HU; WEI, YONG-GANG; (99 pag.)TW2017/8222; (2017); A;,
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