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    • 8. 发明公开
    • PROCESS FOR THE PREPARATION OF PYRAZOLE CARBOXYLIC ACID AMIDES
    • 制备吡唑羧酸酰胺的方法
    • EP2560959A1
    • 2013-02-27
    • EP11714550.8
    • 2011-04-14
    • Syngenta Participations AG
    • DUMEUNIER, RaphaelSCHLETH, FlorianVETTIGER, ThomasROMMEL, MichaelTRAH, Stephan
    • C07D231/14C07D303/17C07C35/52C07C25/24
    • C07D231/14C07C17/23C07C17/30C07C25/24C07C29/132C07C35/52C07C45/29C07C209/10C07C2603/66C07D303/17C07C49/697C07C23/10C07C25/22C07C211/61
    • The invention relates to a process for the preparation of the compound of formula (I), which process comprises a) reacting a compound of formula (II), wherein X is chloro or bromo, with an organometallic species in an inert atmosphere to a halobenzyne of formula (X), reacting the halobenzyne of formula X so formed with cyclopentadiene to (III), b) reacting III in the presence of an inert solvent with an oxidant to (IV), c) reacing IV in the presence of a Lewis acid and a hydride source to (V), d) reacting V in the presence of an oxidizing agent, a base and an inert solvent to (VI), e) converting VI in the presence of a phosphane and CCl
      4 or CHCl
      3 to (VII), and either f1) reacting VII with NH
      3 in the presence of a catalyst to the compound of formula (VIII); and g) reacting VIII in the presence of a base with a compound of formula (IX), to the compound of formula (I); or f2) reacting the compound of formula (VII), in the presence of a solvent, a base, a copper catalyst and at least one ligand with the compound of formula (IXa), to the compound of formula (I).
    • 本发明涉及制备式(I)化合物的方法,该方法包括a)使其中X是氯或溴的式(II)化合物与有机金属物质在惰性气氛中与卤代苄基 (Ⅹ)化合物,使如此形成的式Ⅹ的卤代苄基与环戊二烯与(Ⅲ)反应,b)使Ⅲ在惰性溶剂存在下与氧化剂反应得到(Ⅳ),c)在路易斯 (V),d)使V在氧化剂,碱和惰性溶剂存在下与(VI)反应,e)在磷烷和CCl 4或CHCl 3存在下将VI转化成 (VII)的化合物,并且或者f1)使VII与NH 3在催化剂存在下与式(VIII)的化合物反应; 和g)使VIII在碱存在下与式(IX)化合物反应,得到式(I)化合物; 或f2)使式(VII)化合物在溶剂,碱,铜催化剂和至少一种配体存在下与式(IXa)化合物反应,得到式(I)化合物。