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    • 24. 发明授权
    • Preparation of 6,6'-dihydroxy-3,3,3',3'-tetramethyl-1,1'-spirobiindane
    • 6,6'-二羟基-3,3,3',3'-四甲基-1,1'-螺二茚满的制备
    • US5399783A
    • 1995-03-21
    • US225559
    • 1994-04-11
    • Mizuo ItoShigeru Iimuro
    • Mizuo ItoShigeru Iimuro
    • C07C37/84C07C39/12
    • C07C37/84C07C2103/84
    • Crystals of 6,6'-dihydroxy-3,3,3',3'-tetramethyl -1,1'-spirobiindane (hereinafter referred to as SPI) are obtained by cooling a phenol solution containing 6,6'-dihydroxy-3,3,3',3'-tetramethyl-1,1'-spirobiindane when crystallization is started at a temperature higher than a transition temperature between SPI and an adduct of SPI with phenol. The crystals are washed with an organic solvent or contacted with water and further washed with an organic solvent. When crystallization is started at a temperature less than the transition temperature, adduct crystals of SPI with phenol are obtained from the phenol solution. Phenol is removed from the adduct crystals and the adduct crystals are contacted with water to obtain a hydrate and further the hydrate is washed with an organic solvent.
    • 通过将含有6,6'-二羟基-3,3,3',3'-四甲基-1,1'-螺二茚满的酚溶液(以下称为SPI) ,3,3',3'-四甲基-1,1'-螺二茚满当结晶在高于SPI与SPI与苯酚的加合物之间的转变温度的温度下开始时。 晶体用有机溶剂洗涤或与水接触,并进一步用有机溶剂洗涤。 当在低于转变温度的温度下开始结晶时,从苯酚溶液中获得SPI与苯酚的加合物晶体。 从加合物晶体中除去苯酚,并将加合物晶体与水接触,得到水合物,再用有机溶剂洗涤水合物。
    • 28. 发明授权
    • Process for synthesizing 9,9-bis-(hydroxyphenyl)fluorene
    • 合成9,9-双(羟基苯基)氟的方法
    • US5110994A
    • 1992-05-05
    • US613668
    • 1990-12-10
    • Peter Fialla
    • Peter Fialla
    • B01J27/125C07B61/00C07C37/20C07C37/84C07C39/17
    • C07C39/17C07C37/20C07C2103/18
    • 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.
    • 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。