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    • 8. 发明申请
    • METHOD FOR PREPARING 3-TRIFLUOROMETHYL CHALCONES
    • 制备3-三氟甲基吡咯烷酮的方法
    • WO2009126668A3
    • 2010-04-08
    • PCT/US2009039832
    • 2009-04-08
    • DU PONTANNIS GARY DAVID
    • ANNIS GARY DAVID
    • C07C45/68C07C25/13C07C45/74C07C49/80C07D261/04
    • C07D261/04C07C17/35C07C25/13C07C45/455C07C45/70C07C49/80C07C49/813C07C67/343C07C205/45C07C209/74C07C231/12C07C231/14C07D213/40C07D231/12C07D231/14C07D231/16C07D249/08C07D249/10C07D277/28C07C69/94C07C69/76C07C235/84C07C211/56
    • 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 NR12 R13, 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.
    • 公开了制备式(1)化合物的方法,其中Q和Z如本公开所定义,包括从包含式(2)的化合物,式(3)的化合物,包含 至少一种选自式(4)的碱土金属氢氧化物,其中M是Ca,Sr或Ba的式(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与其中X为Cl,Br或I的式(5)的化合物与镁金属或烷基镁 卤化物,然后(2)使反应混合物与式(6)的化合物(其中Y是OR 11或NR 12 R 13)和R 11,R 12和R 13如本公开中所定义。 进一步公开的是制备式(7)化合物的方法,其中Q和Z如本发明所定义,使用式(1)化合物,其特征在于通过上述方法制备式(1)化合物或使用 通过上述方法制备的式1的化合物。
    • 10. 发明申请
    • 1,3-BIS(TRIFLUOROMETHYL)BENZENE DERIVATIVES
    • 1,3-BIS(三氟甲基)苯并噻吩衍生物
    • WO02024615A1
    • 2002-03-28
    • PCT/GB2001/004258
    • 2001-09-24
    • C07C17/12C07C45/00C07C45/85C07F3/02C07C25/13C07C49/80
    • C07F3/02C07C17/12C07C45/004C07C45/85C07C25/13C07C49/80
    • A method of manufacture of 3,5-bis(trifluoromethyl)bromobenzene, comprising the addition of a brominating reagent to a mixture of 3,5-bis(trifluoromethyl)benzene together with at least one of sulphuric acid or oleum in the absence of acetic acid. A method of production of 3,5-bis(trifluoromethyl)acetophenone comprising the reaction of 3,5-bis(trifluoromethyl)phenyl magnesium bromide with acetyl chloride in the presence of cuprous chloride. A method of production of 3,5-bis(trifluoromethyl)acetophenone comprising the steps of reacting 3,5-bis(trifluoromethyl)phenyl magnesium bromide with acetic anhydride, adding water, and recovering the product by azeotropic distillation. A method of removal of impurities including 3,5-bis(trifluoromethyl)acetate, 4-bromobutyl acetate and 4-chlorobutyl acetate from a preparation of 3,5-bis(trifluoromethyl)acetophenone, the method comprising heating the 3,5-bis(trifluoromethyl)acetophenone with a dilute solution of alkali. A method of production of 3,5-bis(trifluoromethyl)phenyl magnesium bromide comprising the reaction of 3,5-bis(trifluoromethyl)bromobenzene with magnesium in a solvent whilst maintaining the temperature of the reactants above 20 DEG C and below the reflux temperature of the solvent.
    • 制备3,5-二(三氟甲基)溴苯的方法,包括在不存在乙酸的情况下向3,5-二(三氟甲基)苯与硫酸或发烟硫酸中的至少一种加入溴化试剂 酸。 包括3,5-二(三氟甲基)苯基溴化镁与乙酰氯在氯化亚铜存在下反应的3,5-二(三氟甲基)苯乙酮的生产方法。 制备3,5-双(三氟甲基)苯乙酮的方法,包括使3,5-二(三氟甲基)苯基溴化镁与乙酸酐反应,加水并通过共沸蒸馏回收产物的步骤。 从3,5-双(三氟甲基)苯乙酮的制备物中除去包括3,5-双(三氟甲基)乙酸酯,乙酸4-溴丁酯和乙酸4-氯丁酯的杂质的方法,该方法包括加热3,5-二 (三氟甲基)苯乙酮与稀碱溶液。 包括3,5-二(三氟甲基)苯基溴化镁的生产方法,包括在溶剂中3,5-二(三氟甲基)溴苯与镁的反应同时保持反应物的温度高于20℃并低于回流温度 的溶剂。