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    Method for producing fluorene derivative
    7.
    发明申请
    Method for producing fluorene derivative 审中-公开
    芴衍生物的制备方法

    公开(公告)号：US20070100170A1

    公开(公告)日：2007-05-03

    申请号：US10501890

    申请日：2002-01-29

    申请人： Hiroaki Murase ,  Mitsuaki Yamada ,  Yasuhiro Suda ,  Kazuyuki Ogata

    发明人： Hiroaki Murase ,  Mitsuaki Yamada ,  Yasuhiro Suda ,  Kazuyuki Ogata

    IPC分类号： C07C43/20 ,  C07C39/12

    CPC分类号： C07C37/20 ,  C07C2603/18 ,  C07C39/17

    摘要： Fluorenone and a phenolic compound (e.g., a 2-C1-4alkylphenol) is subjected to a condensation reaction in coexistence with a thiol compound and a hydrochloric acid aqueous solution to produce a fluorene derivative [e.g., 9,9-bis(C1-4alkylhydroxyphenyl)fluorene]. The proportion (weight ratio) of fluorenone relative to the thiol compound [fluorenone/the thiol compound] is about 1/0.01 to 1/0.5, and the proportion (weight ratio) of the thiol compound relative to hydrochloric acid (HCl) in the hydrochloric acid aqueous solution [the thiol compound/hydrochloric acid] is about 1/0.1 to 1/3. As the thiol compound, a mercaptocarboxylic acid (β-mercaptopropionic acid) may be used. According to the method, a highly purified fluorene derivative excellent in transparency can be obtained inexpensively and simply without using a hydrogen chloride gas having handling difficulty.

    摘要翻译： 芴酮和酚类化合物（例如2-C 1-4烷基酚）与硫醇化合物和盐酸水溶液共存以进行缩合反应，生成芴衍生物[例如， 9,9-双（C 1-4烷基羟基苯基）芴]。 芴酮相对于硫醇化合物[芴酮/硫醇化合物]的比例（重量比）为约1 / 0.01〜1 / 0.5，硫醇化合物相对于盐酸（HCl）的比例（重量比）为 盐酸水溶液[硫醇化合物/盐酸]为约1 / 0.1〜1/3。 作为硫醇化合物，可以使用巯基羧酸（β-巯基丙酸）。 根据该方法，可以廉价且简单地获得透明性优异的芴衍生物，而不使用具有处理难度的氯化氢气体。

    Method of preparing a fluorene derivative and the method of purifying thereof
    8.
    发明授权
    Method of preparing a fluorene derivative and the method of purifying thereof 失效
    芴衍生物的制备方法及其纯化方法

    公开(公告)号：US5629456A

    公开(公告)日：1997-05-13

    申请号：US350459

    申请日：1994-12-07

    申请人： Mitsuaki Yamada ,  Katsuhide Okimi ,  Katsuyuki Takahashi ,  Norio Nagano

    发明人： Mitsuaki Yamada ,  Katsuhide Okimi ,  Katsuyuki Takahashi ,  Norio Nagano

    IPC分类号： B01J31/02 ,  C07B61/00 ,  C07C41/30 ,  C07C41/40 ,  C07C43/23 ,  C07C39/12

    CPC分类号： C07C43/23 ,  C07C2103/18

    摘要： A fluorene derivative of high purity is produced by reacting fluorenone with phenoxyethanol in the presence of a sulfuric acid-thiol catalyst system, dissolving the reaction mixture in a lower aliphatic alcohol and adding water to the resulting solution for precipitation of 9,9-bis(4-(2-hydroxyethoxy)phenyl)fluorene [fluorene derivative]. A fluorene derivative of still higher purity is obtained by recrystallization from a lower aliphatic alcohol.In accordance with this invention, a fluorene derivative can be produced advantageously on a commercial scale without incurring any appreciable loss of fluorenone, in good yield, with high efficiency and in a reduced production time.

    摘要翻译： 通过在硫酸 - 硫醇催化剂体系的存在下使芴酮与苯氧基乙醇反应制备高纯度的芴衍生物，将反应混合物溶解在低级脂族醇中，向所得溶液中加入9,9-双（ 4-（2-羟基乙氧基）苯基）芴[芴衍生物]。 通过从低级脂族醇重结晶获得更高纯度的芴衍生物。 根据本发明，可以以商业规模有利地生产芴衍生物，而不会以良好的产率，高效率和缩短的生产时间引起芴酮的明显损失。