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approach to the synthesis of 9,9-bis (4 - hydroxyphenyl) fluorene

机译:9,9-双(4-羟基苯基)芴的合成方法

摘要

PCT No. PCT/AT90/00031 Sec. 371 Date Dec. 10, 1990 Sec. 102(e) Date Dec. 10, 1990 PCT Filed Apr. 17, 1990 PCT Pub. No. WO90/12776 PCT Pub. Date Nov. 1, 1990.The invention concerns a process for synthesizing 9,9-bis(hydroxyphenyl)fluorene by reacting fluorene with excess phenol using a liquid catalyst prepared by dissolving aluminum trichloride in an anhydrous organic solvent such as toluene evincing the property of an electron donor while hydrochloric-acid gas is being supplied. For the purpose of the synthesis, the fluorenone is dissolved for instance at 60 DEG C. in the liquid phenol and then the liquid catalyst is dripped into the agitated reaction mixture at such a rate that the temperature of the reaction mixture is kept below 60 DEG C. Following catalyst addition and subsequent after-reaction interval of several hours, the raw product is mixed with hot water and the excess phenol is removed by steam distillation. After signle-washing with water, the raw product is dissolved in hot acetone, allowed to crystallize, is filtered out and dried in vacuum. Lastly the raw product is recrystallized from 1,2-dichloroethane to form the pure product.
机译:PCT号PCT / AT90 / 00031秒371日期1990年12月10日102(e),1990年12月10日,PCT,1990年4月17日提交,PCT公开。 WO90 / 12776 PCT公开号日期为1990年11月1日。本发明涉及一种通过使用使三氯化铝溶解在无水有机溶剂如甲苯中的液体催化剂使芴与过量的苯酚反应来合成9,9-双(羟基苯基)芴的方法,该方法证明了氯的性能。在供应盐酸气体的同时提供电子给体。为了合成,将芴酮例如在60℃下溶解在液体苯酚中,然后以使反应混合物的温度保持在60℃以下的速率将液体催化剂滴入搅拌的反应混合物中。在添加催化剂和随后的数小时的后反应间隔之后,将粗产物与热水混合,并通过蒸汽蒸馏除去过量的苯酚。用水洗净后,将粗产物溶于热丙酮中,使其结晶,过滤并真空干燥。最后,将粗产物从1,2-二氯乙烷中重结晶以形成纯产物。

著录项

  • 公开/公告号DK0419631T3

    专利类型

  • 公开/公告日1993-10-04

    原文格式PDF

  • 申请/专利权人 ISONOVA TECHNISCHE INNOVATIONEN GES.M.B.H.;

    申请/专利号DK19900906045T

  • 发明设计人 FIALLA PETER;

    申请日1990-04-17

  • 分类号C07C37/20;C07C39/17;

  • 国家 DK

  • 入库时间 2022-08-22 05:12:09

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