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    • 9. 发明授权
    • Method for preparing 3-trifluoromethyl chalcones
    • 制备3-三氟甲基查尔酮的方法
    • US09035101B2
    • 2015-05-19
    • US14041938
    • 2013-09-30
    • E.I. du Pont de Nemours and Company
    • Gary David Annis
    • C07C45/70C07C49/80C07C17/35C07C25/13C07C67/343C07C205/45C07C231/12C07D213/40C07D249/08C07D249/10C07D261/04C07D277/28C07C209/74C07C45/45
    • C07D261/04C07C17/35C07C25/13C07C45/455C07C45/70C07C49/80C07C49/813C07C67/343C07C205/45C07C209/74C07C231/12C07C231/14C07C235/84C07D213/40C07D231/12C07D231/14C07D231/16C07D249/08C07D249/10C07D277/28C07C69/94C07C69/76C07C211/56
    • Disclosed is a method for preparing a compound of Formula 1 wherein Q and Z are as defined in the disclosure comprising distilling water from a mixture comprising a compound of Formula 2, a compound of Formula 3, a base comprising at least one compound selected from the group consisting of alkaline earth metal hydroxides of Formula 4 wherein M is Ca, Sr or Ba, alkali metal carbonates of Formula 4a wherein M1 is Li, Na or K, 1,5-diazabicyclo[4.3.0]non-5-ene and 1,8-diazabicyclo[5.4.0]undec-7-ene, and an aprotic solvent capable of forming a low-boiling azeotrope with water. Also disclosed is a method for preparing a compound of Formula 2 comprising (1) forming a reaction mixture comprising a Grignard reagent derived from contacting a compound of Formula 5 wherein X is Cl, Br or I with magnesium metal or an alkylmagnesium halide in the presence of an ethereal solvent, and then (2) contacting the reaction mixture with a compound of Formula 6 wherein Y is OR11 or NR12R13, and R11, R12 and R13 are as defined in the disclosure. Further disclosed is a method for preparing a compound of Formula 7 wherein Q and Z are as defined in the disclosure, using a compound of Formula 1 characterized by preparing the compound of Formula 1 by the method disclosed above or using a compound of Formula 1 prepared by the method disclosed above.
    • 公开了一种制备式1化合物的方法,其中Q和Z如本公开中所定义,包括从包含式2化合物,式3化合物,包含至少一种选自 由式4的碱土金属氢氧化物组成的组,其中M是Ca,Sr或Ba,式4a的碱金属碳酸盐,其中M1是Li,Na或K,1,5-二氮杂双环[4.3.0]壬-5-烯和 1,8-二氮杂双环[5.4.0]十一碳-7-烯,以及能够与水形成低沸点共沸物的非质子传递溶剂。 还公开了制备式2化合物的方法,其包括(1)形成反应混合物,该反应混合物包含衍生自在存在下使式5的化合物(其中X为Cl,Br或I)与镁金属或烷基卤化镁接触的格利雅试剂 的醚溶剂,然后(2)使反应混合物与式6化合物(其中Y是OR 11或NR 12 R 13)和R 11,R 12和R 13如本公开所定义。 进一步公开的是制备式7化合物的方法,其中Q和Z如本公开所定义,使用式1的化合物,其特征在于通过上述方法制备式1化合物或使用制备的式1化合物 通过上述方法。