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1. 发明授权

US5110994A Process for synthesizing 9,9-bis-(hydroxyphenyl)fluorene 失效
标题翻译：合成9,9-双（羟基苯基）氟的方法
公开(公告)号：US5110994A
公开(公告)日：1992-05-05
申请号：US613668
申请日：1990-12-10
申请人： Peter Fialla
发明人： Peter Fialla
IPC分类号： B01J27/125 , C07B61/00 , C07C37/20 , C07C37/84 , C07C39/17
CPC分类号： C07C39/17 , C07C37/20 , C07C2103/18
摘要： 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.degree. 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.degree. 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.
摘要翻译： PCT No.PCT / AT90 / 00031 Sec。 371 1990年12月10日第 102（e）1990年12月10日日期PCT提交1990年4月17日PCT公布。 WO90 / 12776 PCT出版物日本1990年11月1日。本发明涉及通过使用通过将三氯化铝溶解在无水有机溶剂如甲苯中制备的液体催化剂使芴与过量苯酚反应来合成9,9-双（羟基苯基）芴的方法，电子给体，同时供应盐酸气体。为了合成的目的，将芴酮例如在60℃下溶解在液体苯酚中，然后将液体催化剂滴入搅拌的反应混合物中，使反应混合物的温度保持在60℃以下 C.催化剂加入和随后的反应间隔数小时后，将原料与热水混合，通过蒸汽蒸馏除去过量的苯酚。用水标志洗涤后，将粗产物溶于热丙酮中，使其结晶，过滤并真空干燥。最后，将原料从1,2-二氯乙烷中重结晶形成纯产物。

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