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    • 3. 发明公开
    • Process for preparing 2,4,5-trifluorobenzoic acid
    • 制备2,4,5-三氟苯甲酸的方法
    • EP0385253A1
    • 1990-09-05
    • EP90103334.0
    • 1990-02-21
    • OCCIDENTAL CHEMICAL CORPORATION
    • Lin, Henry C.Nowak, Deanne M.
    • C07C63/70C07C51/363
    • C07C51/363C07C227/18C07C245/20C07C63/70C07C229/56
    • 2,4,5-Trifluorobenzoic acid is prepared by converting 4,5-di­fluoroanthranilic acid to the corresponding amine salt, converting the amine salt to the corresponding diazonium tetrafluoroborate and decomposing the tetrafluoroborate in a Schiemann reaction. In a preferred preparation, the 10 percent HCl is added to solid 4,5-difluoroanthranilic acid in sufficient amount to dissolve the solid at 70°C, the amine salt is isolated, aqueous NaNO₂ is added to the isolated amine salt at 0°C, followed by addition of 40 to 50 percent aqueous HBF₄ at 0°C, followed by separation of the tetra­fluoroborate by cooling and filtering and then drying, and the dried separated tetrafluoroborate is thermally degraded to 2,4,5-­trifluorobenzoic acid by heating at 125 to 140°C.
    • 通过将4,5-二氟邻氨基苯甲酸转化为相应的胺盐,将胺盐转化为相应的重氮四氟硼酸盐并在Schiemann反应中分解四氟硼酸盐来制备2,4,5-三氟苯甲酸。 在一个优选的制备中,将10%HCl加到固体4,5-二氟邻氨基苯甲酸中,其量足以在70℃下溶解固体,分离出胺盐,在0℃下将NaNO 2水溶液加入分离的胺盐 ,然后在0℃下加入40-50%的HBF 4水溶液,接着通过冷却和过滤分离四氟硼酸盐,然后干燥,干燥的分离出的四氟硼酸盐通过加热到250℃热分解成2,4,5-三氟苯甲酸 125至140°C。