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    • 1. 发明授权
    • Process for preparing 4,4'-dihydroxydiphenyl sulfone having high purity
    • 制备高纯度的4,4'-二羟基二苯砜的方法
    • US4820831A
    • 1989-04-11
    • US10095
    • 1986-12-12
    • Eiji OgataKoji OnoNobuyuki Nate
    • Eiji OgataKoji OnoNobuyuki Nate
    • C07C315/00B01J31/02C07C67/00C07C313/00C07C317/22F15B11/04C07C147/10
    • C07C317/00
    • The process of the present invention is a process for preparing 4,4'-dihydroxydiphenyl sulfone by subjecting phenol, and a sulfonating agent or phenolsulfonic acid to a dehydration reaction in the presence of a solvent, subsequently maintaining the reaction system at a temperature of between 100.degree. to 200.degree. C. and removing the solvent from the reaction system to cause the dehydration reaction to further proceed while allowing 4,4'-dihydroxydiphenyl sulfone to separate out and to subject dissolved 2,4'-dihydroxydiphenyl sulfone formed as a by-product to an isomerization reaction for converting the by-product to 4,4'-dihydroxydiphenyl sulfone, and eventually removing the solvent and the unreacted phenol from the system substantially entirely to complete the isomerization reaction, the process being characterized in that an aromatic sulfonic acid represented by the formula ##STR1## wherein X is a halogen atom, n is 0, 1 or 2, and m is 1 of 2 is caused to be present in the reaction system. 4,4'-Dihydroxydiphenyl sulfone can be produced by the process with a high purity and in a high yield.
    • PCT No.PCT / JP86 / 00194 Sec。 371日期:1986年12月12日 102(e)日期1986年12月12日PCT提交1986年4月17日PCT公布。 公开号WO86 / 06370 日本1986年11月6日。本发明的方法是通过在溶剂存在下使苯酚和磺化剂或苯酚磺酸进行脱水反应来制备4,4'-二羟基二苯基砜的方法, 反应体系在100〜200℃的温度下,从反应体系中除去溶剂,使脱水反应进一步进行,同时使4,4'-二羟基二苯砜分离出来并使溶解的2,4' - 二羟基二苯砜作为副产物形成异构化反应,用于将副产物转化为4,4'-二羟基二苯基砜,并最终从体系中除去溶剂和未反应的苯酚,完全完全异构化反应,该方法 其特征在于,由式“IMAGE”表示的芳族磺酸,其中X为卤素原子,n为0,1或2,m为2的m为芳族磺酸存在于 反应体系。 4,4'-二羟基二苯砜可以通过高纯度和高收率的方法生产。
    • 3. 发明授权
    • Process for producing 4,4'-dihydroxydiphenylsulfone of high purity
    • 生产高纯度的4,4'-二羟基二苯基砜的方法
    • US4162270A
    • 1979-07-24
    • US896611
    • 1978-04-14
    • Eiji OgataKoji OnoShoji Nakagaki
    • Eiji OgataKoji OnoShoji Nakagaki
    • C07C315/00C07C317/22C07C147/10
    • C07C315/00
    • In a process for producing 4,4'-dihydroxydiphenylsulfone by reacting phenol with sulfuric acid in the presence of a solvent, an improvement which comprises using at least a member selected from the group consisting of chlorobenzene, dichlorobenzene, trichlorobenzene, chlorotoluene, diethylbenzene, xylene, decalin, tetralin and tetrachloroethane as the solvent and removing said solvent progressively and finally substantially completely from the mixture while maintaining the reaction mixture at a temperature of about 160.degree. to about 200.degree. C. to effect precipitation of 4,4'-dihydroxydiphenylsulfone and isomerization of 2,4'-dihydroxydiphenylsulfone to 4,4'-dihydroxydiphenylsulfone.
    • 在溶剂存在下,通过苯酚与硫酸反应生产4,4'-二羟基二苯砜的方法,包括使用至少一种选自氯苯,二氯苯,三氯苯,氯甲苯,二乙苯,二甲苯 ,十氢化萘,四氢化萘和四氯乙烷作为溶剂,并逐渐地并最终基本上完全从混合物中除去所述溶剂,同时将反应混合物保持在约160℃至约200℃的温度,以实现4,4'-二羟基二苯砜和 2,4'-二羟基二苯砜异构化为4,4'-二羟基二苯砜。
    • 4. 发明授权
    • Process for purifying 4,4'-dihydroxydiphenylsulfone
    • 纯化4,4'-二羟基二苯基砜的方法
    • US5097074A
    • 1992-03-17
    • US362411
    • 1989-04-10
    • Eiji OgataKoji Ono
    • Eiji OgataKoji Ono
    • C07C315/06C07C317/22C07C317/24
    • C07C315/06
    • The invention provides a process for purifying crude 4,4'-dihydroxydiphenylsulfone characterized by dissolving the crude 4,4'-dihydroxydiphenylsulfone in an aqueous solution of a basic substance, precipitating a mono-salt of 4,4'-dihydroxydiphenylsulfone from the resulting solution by salting out, separating the salt off and subsequently treating the salt with an acid, and also porovides a process for preparing a mono-salt of 4,4'-dihydroxydiphenylsulfone characterized by dissolving crude 4,4'-dihydroxydiphenylsulfone in an aqueous solution of a basic substance, precipitating a mono-salt of 4,4'-dihydroxydiphenylsulfone from the resulting solution by salting out, and separating the salt off.
    • PCT No.PCT / JP88 / 00813 Sec。 371日期:1989年4月10日 102(e)日期1989年4月10日PCT提交1988年8月17日PCT公布。 出版物WO89 / 01469 日本特开1989年2月23日。本发明提供一种纯化粗制4,4'-二羟基二苯砜的方法,其特征在于将粗制4,4'-二羟基二苯砜溶于碱性物质的水溶液中,沉淀出4,4'-二羟基二苯砜的单盐 通过盐析从所得溶液中分离出脱盐并随后用酸处理盐,并且还可以制备4,4'-二羟基二苯基砜单盐的方法,其特征在于将粗4,4'-二羟基二苯砜 - 二羟基二苯砜在碱性物质的水溶液中,通过盐析从所得溶液中沉淀出4,4'-二羟基二苯砜的单盐,并将盐分离。
    • 5. 发明申请
    • Multilayer wiring substrate
    • 多层布线基板
    • US20080227312A1
    • 2008-09-18
    • US12076014
    • 2008-03-12
    • Eiji OgataKazunori OmoriKoichi NamimatsuKazunari Fukagawa
    • Eiji OgataKazunori OmoriKoichi NamimatsuKazunari Fukagawa
    • H01R12/06
    • H05K3/4046H05K3/3447H05K2201/0133H05K2201/09645H05K2201/1059
    • A first wiring pattern formed on a first layer of a multilayer wiring substrate, a second wiring pattern formed on a layer different from the first layer on which the first wiring pattern is formed, a penetration hole penetrating the front surface and the back surface of the substrate, and a penetration hole penetrating a front surface and a back surface of the substrate; and a fitting connector having a conductor part on a side surface inscribed in the penetration hole and fitting into the penetration hole are provided. The first wiring pattern and the second wiring pattern are exposed from the internal surface of the penetration hole, and the fitting connector connects a first end part of the conductor part and a second end part with an exposed part of the first wiring pattern and an exposed part of the second wiring pattern, respectively.
    • 形成在多层布线基板的第一层上的第一布线图案,形成在与形成有第一布线图案的第一层不同的层上的第二布线图案,穿透第一布线图案的前表面和后表面的穿透孔 基板和穿透基板的前表面和后表面的穿透孔; 以及配合连接器,其具有位于贯通孔内侧的嵌合于贯通孔的侧面的导体部。 第一布线图案和第二布线图案从穿孔的内表面露出,并且嵌合连接器将导体部的第一端部和第二端部与第一布线图案的露出部分连接, 分别是第二布线图案的一部分。
    • 9. 发明授权
    • Highly purified tocopheryl phosphate, process for producing the same,
analytical method therefor and cosmetic
    • 高纯度生育磷酸酯,其生产方法,分析方法和化妆品
    • US6046181A
    • 2000-04-04
    • US342228
    • 1999-06-29
    • Yutaka OonishiTsutomu NozawaTakami OoeKeisuke ManoNaoaki MisuYohei KurataShinobu ItoEiji Ogata
    • Yutaka OonishiTsutomu NozawaTakami OoeKeisuke ManoNaoaki MisuYohei KurataShinobu ItoEiji Ogata
    • A61K8/02A61K8/67A61Q1/02A61Q1/04A61Q5/02A61Q7/00A61Q11/00A61Q19/00A61Q19/10C07F9/655G01N30/02G01N30/88G01N33/82A61K7/035A61K7/00A61K7/02A61K7/021A61K7/027
    • G01N33/82A61K8/0212A61K8/678A61Q19/00C07F9/65522A61Q1/02A61Q1/04A61Q11/00A61Q19/10A61Q5/02A61Q7/00G01N2030/884G01N30/02Y10S514/846
    • Disclosed herein are a highly purified tocopheryl phosphate and/or a salt thereof (tocopheryl phosphates) wherein a P,P'-bistocopheryl hypophosphate and/or a salt thereof (P,P'-bistocopheryl diphoshates) is contained in a proportion of not higher than 3% by weight; a process for producing a highly purified tocopheryl phosphate and/or a salt thereof, which comprises the steps of reacting a tocopherol with an oxyphosphorus trihalide followed by treating with an acid or basic aqueous solution to thereby form tocopheryl phosphates (i) in which P,P'-bistocopheryl diphoshates (ii) formed as by-products are contained, hydrolyzing the P,P'-bistocopheryl diphoshates (ii) under acid condition, and, optionally, rendering the hydrolyzate neutral or basic under basic condition; and a method of analyzing tocopheryl phosphates, comprising analyzing a sample containing components (i) and (ii) with the use of a high-performance liquid chromatograph column packed with a gel of a polymethacrylate having, bonded thereto, long-chain alkyl groups. None or only an extremely minute amount of P,P'-bistocopheryl diphoshates are contained in the highly purified tocopheryl phosphates, so that the highly purified tocopheryl phosphates exhibit antioxidant and blood circulation promoting effects, have excellent water solubility, are powdery so that the handling thereof is extremely easy, are free from cutaneous irritation and allergenecity and ensure dermal safety. Therefore, the highly purified tocopheryl phosphates are useful as cosmetic ingredients. The amounts of components (i) and (ii) can be simply measured with high accuracy by the above method.
    • 本文公开了高纯度的生育磷酸酯和/或其盐(生育磷酸酯),其中P,P'-二生育酚低磷酸盐和/或其盐(P,P'-二生育基二磷酸酯)的含量不高于 超过3%重量; 一种生产高纯度生育磷酸酯和/或其盐的方法,其包括使生育酚与三卤氧磷反应,然后用酸或碱性水溶液处理,从而形成生育磷酸酯(i),其中P, 含有作为副产物形成的P'-二生育基二磷酸酯(ⅱ),在酸性条件下水解P,P'-二生育基二磷酸酯(ⅱ),任选地在碱性条件下使水解产物中性或碱性。 以及分析生育磷酸酯的方法,包括使用填充有与其键合的聚甲基丙烯酸酯的凝胶的高效液相色谱柱分析含有成分(i)和(ii)的样品的长链烷基。 高纯度的生育磷酸酯中没有或仅有非常少量的P,P'-二生育基二磷酸酯,因此高纯度的生育磷酸酯表现出抗氧化和促进血液循环的作用,具有优异的水溶性,是粉末状的, 它非常容易,没有皮肤刺激和过敏原,并确保皮肤安全。 因此,高纯度的生育磷酸酯可用作化妆品成分。 组分(i)和(ii)的量可以通过上述方法以高精度简单地测量。