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    • 4. 发明授权
    • Process for preparing [bis-(trifluoromethyl)-phenyl]-acetic acids and alkyl esters thereof and dialkyl [bis-(trifluoromethyl)-phenyl]-malonates
    • 制备[双(三氟甲基) - 苯基] - 乙酸及其烷基酯和[双(三氟甲基) - 苯基] - 丙二酸二烷基酯的方法
    • US06395921B1
    • 2002-05-28
    • US09635164
    • 2000-08-09
    • Albrecht MarholdJörn Stölting
    • Albrecht MarholdJörn Stölting
    • C07C6976
    • C07C69/65C07C51/38C07C67/32C07C67/343C07C57/58
    • [Bis-(trifluoromethyl)-phenyl]-acetic acids are obtained in an advantageous manner by reacting an appropriate bromo- or iodo-bis-(trifluoromethyl)-benzene with a di-C1-C4-alkyl malonate in the presence of a deprotonating agent and a copper salt and hydrolysing and decarboxylating the reaction product in basic medium. It is possible to obtain a mixture of alkyl [bis-(trifluoromethyl)-phenyl]-acetate and alkyl [bis-(tri-fluoromethyl)-phenyl]-malonate by admixing the reaction mixture which is present before hydrolysis and complete decarboxylation with water and acid and heating. From the mixture, it is possible to obtain alkyl [bis-(trifluoromethyl)-phenyl]-acetate by distillation under reduced pressure and dialkyl [bis-(trifluoromethyl)-phenyl]-malonate by work-up by column chromatography, fractional distillation or film distillation. [Bis-(trifluoromethyl)-phenyl]-malonic esters are novel compounds.
    • 通过使合适的溴 - 或碘 - 双 - (三氟甲基) - 苯与二-C1- C4烷基丙二酸酯在去质子化反应的存在下,通过有利的方式获得[双(三氟甲基) - 苯基] - 乙酸 试剂和铜盐,并在碱性介质中水解和脱羧反应产物。 可以通过将水解之前存在的反应混合物与水完全脱羧反应获得[双((三氟甲基) - 苯基] - 乙酸烷基酯和[双 - (三氟甲基) - 苯基] - 丙二酸烷基酯的混合物 酸和加热。 从混合物中,可以通过在柱下色谱法,分馏或后处理中减压蒸馏和[双(三氟甲基) - 苯基] - 丙二酸二烷基酯来获得[双(三氟甲基) - 苯基] [双(三氟甲基) - 苯基] - 丙二酸酯是新化合物。
    • 7. 发明授权
    • Process for the preparation of 3,5-bis(trifluoro-methyl)-benzoyl chlorides and novel 3,5-bis(tri-halogenomethyl)-and 3,5-dimethylbenzoyl halides
    • 制备3,5-二(三氟 - 甲基) - 苯甲酰氯和新的3,5-双(三卤代甲基) - 和3,5-二甲基苯甲酰基卤化物的方法
    • US06420601B2
    • 2002-07-16
    • US09769797
    • 2001-01-25
    • Albrecht MarholdJörn Stölting
    • Albrecht MarholdJörn Stölting
    • C07C5158
    • C07C51/60C07C51/62C07C63/70C07C63/72
    • 3,5-Bis(trifluoromethyl)benzoyl chlorides optionally substituted with fluorine or chlorine are advantageously prepared by converting 3,5-dimethylbenzoic acids optionally substituted with fluorine or chlorine into the corresponding acid chlorides; completely free-radically chlorinating said chlorides in the side chains, giving 3,5-bis(trichloromethyl)benzoyl chlorides optionally substituted by fluorine or chlorine; fluorinating the latter with anhydrous hydrogen fluoride and/or antimony pentafluoride, giving 3,5-bis(trifluoromethyl)benzoyl fluorides optionally substituted with fluorine or chlorine; and then reacting the 3,5-bis(trifluoromethyl)benzoyl fluorides with silicon tetrachloride in the presence of a further Lewis acid. Some of the 3,5-bis(trihalogenomethyl) and 3,5-dimethylbenzoyl halides which arise as intermediates are novel compounds.
    • 任选被氟或氯取代的3,5-双(三氟甲基)苯甲酰氯有利地通过将任选被氟或氯取代的3,5-二甲基苯甲酸转化成相应的酰氯来制备; 完全自由基地氯化侧链中的氯化物,得到任选被氟或氯取代的3,5-双(三氯甲基)苯甲酰氯; 用无水氟化氢和/或五氟化锑氟化后者,得到任选被氟或氯取代的3,5-双(三氟甲基)苯甲酰氟; 然后在另外的路易斯酸的存在下使3,5-双(三氟甲基)苯甲酰氟与四氯化硅反应。 作为中间体产生的一些3,5-二(三卤代甲基)和3,5-二甲基苯甲酰基卤化物是新的化合物。