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    • 39. 发明专利
    • Production of 3-chloro-4-fluorobenzotrifluoride
    • 生产3-氯-4-氟荧光素
    • JPS61126042A
    • 1986-06-13
    • JP24616884
    • 1984-11-22
    • Asahi Glass Co Ltd
    • KUMAI SEISAKUSEKI TAKASHIMATSUO HITOSHI
    • C07C17/20B01J27/00B01J27/12C07B61/00C07C17/00C07C17/093C07C25/13C07C67/00
    • Y02P20/52
    • PURPOSE: To produce the titled substance in high purity and yield, by substituting a 4-halogene-3-nitrobenzotrifluoride with fluorine using a metal fluoride, and reacting with chlorine gas to effect the substitution of the nitro group with chlorine.
      CONSTITUTION: The objective compound of formula III can be produced by (1) reacting the compound of formula I (X is Cl or Br) with a metal fluoride such as KF in an aprotic polar solvent (preferably sulfolane) at 130W160°C and 1W20kg/cm
      2 for 1W30hr to obtain the compound of formula II, (2) distilling the reaction liquid optionally after separating the unreacted metal fluoride by filtration, and (3) reacting the compound of formula II separated by the step 2 with chlorine gas at 150W350°C and 3W15kg/cm
      2 for 2W30hr. The chlorine-substitution reaction of the nitro group is preferably carried out in the presence of an HF-trapping agent (e.g., CaCl
      2 ) and/or a dehydration agent (e.g. SbCl
      5 ).
      USE: Intermediate of pharmaceuticals and agricultural chemicals.
      COPYRIGHT: (C)1986,JPO&Japio
    • 目的:通过使用金属氟化物用氟代替4-卤代-3-硝基三氟甲苯,与氯气反应,用氯代替硝基,制备高纯度和收率的标题物质。 结构式:式III的目标化合物可以通过以下步骤制备:(1)使式I化合物(X为Cl或Br)与金属氟化物如KF在非质子极性溶剂(优选环丁砜)中在130-160℃下反应。 C和1-20kg / cm 2反应1-30小时,得到式II化合物,(2)任选地在过滤分离未反应的金属氟化物之后蒸馏反应液,和(3)使分离的式II化合物 通过步骤2,在150-350℃的氯气和3-15kg / cm 2下2-30小时。 硝基的氯取代反应优选在HF捕获剂(例如CaCl 2)和/或脱水剂(例如SbCl 5)的存在下进行。 用途:药物和农药中间体。