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    Conversion of perylene-3,4:9,10-tetracarboximides to a form suitable for use as fluorescent dyes
    1.
    发明授权
    Conversion of perylene-3,4:9,10-tetracarboximides to a form suitable for use as fluorescent dyes 有权
    将苝-3,4：9,10-四羧酰亚胺转化为适合用作荧光染料的形式

    公开(公告)号：US07851628B2

    公开(公告)日：2010-12-14

    申请号：US12346262

    申请日：2008-12-30

    申请人： Peter Erk ,  Simone Schaefer ,  Arno Boehm ,  Peter Blaschka ,  Harald Arms ,  Willi Helfer

    发明人： Peter Erk ,  Simone Schaefer ,  Arno Boehm ,  Peter Blaschka ,  Harald Arms ,  Willi Helfer

    IPC分类号： C09B3/14 ,  C07D471/00

    CPC分类号： C09B67/0014 ,  C09B67/0025

    摘要： A process for converting perylene-3,4:9,10-tetracarboximides of the general formula I in which R1 and R2 are each unbranched, branched or cyclic C1-C8-alkyl to a form suitable for use as fluorescent dyes, which comprises a) dissolving or suspending the perylene-3,4:9,10-tetracarboximides whose molecules have a molecular volume of ≦230 Å3 in an organic or inorganic solvent at from 0 to 250° C., b1) cooling the solution obtained in step a) to or below the crystallization temperature and, in the case of an organic solvent, if desired at the same time removing excess solvent until the first crystals form, or, in the case of an inorganic solvent, adding water or dilute aqueous solutions of the solvent until the first crystals form, and maintaining the solution at this temperature for further crystallization or b2) cooling the suspension obtained in step a) to or below the crystallization temperature when the temperature in step a) was above the crystallization temperature, and maintaining the suspension at this temperature for further crystallization, c) isolating the solvate crystals formed in step b) and d) then removing the solvent from the solvate crystals, and also novel crystalline forms of perylene-3,4:9,10-tetracarboxylic diimides.

    摘要翻译： 用于将通式I的苝-3,4：9,10-四甲酰亚胺转化为其中R 1和R 2各自是非支链，支链或环状的C 1 -C 8烷基的方法，其适于用作荧光染料，其包含 ）在有机或无机溶剂中在0至250℃下溶解或悬浮其分子具有分子量为＆amp; 230;Å3的苝-3,4：9,10-四甲酰亚胺，b1）冷却步骤 a）达到或低于结晶温度，并且在有机溶剂的情况下，如果需要，同时除去过量的溶剂直到形成第一晶体，或者在无机溶剂的情况下，加入水或稀的水溶液 溶剂直到形成第一晶体，并将溶液保持在该温度下进一步结晶，或b2）当步骤a）中的温度高于结晶温度时，将步骤a）中获得的悬浮液冷却至或低于结晶温度，并将其固化 在该温度下搅拌悬浮液进一步结晶，c）分离步骤b）中形成的溶剂化物晶体，d）然后从溶剂合物晶体中除去溶剂，还可以形成苝-3,4：9,10-四羧酸 二酰亚胺

    Method for converting perylen-3,4:9,10-tetracarboxylic acid diimides into a form suitable for use as a fluorescent dye
    2.
    发明授权
    Method for converting perylen-3,4:9,10-tetracarboxylic acid diimides into a form suitable for use as a fluorescent dye 有权
    将苝-3,4：9,10-四羧酸二酰亚胺转化为适合用作荧光染料的形式的方法

    公开(公告)号：US07753967B2

    公开(公告)日：2010-07-13

    申请号：US10514564

    申请日：2003-06-06

    申请人： Peter Erk ,  Simone Schaefer ,  Arno Boehm ,  Peter Blaschka ,  Harald Arms ,  Willi Helfer

    发明人： Peter Erk ,  Simone Schaefer ,  Arno Boehm ,  Peter Blaschka ,  Harald Arms ,  Willi Helfer

    IPC分类号： C09B3/14 ,  C07B63/00

    CPC分类号： C09B67/0014 ,  C09B67/0025

    摘要： Novel crystalline forms of and a process for converting perylene-3,4:9,10-tetracarboximide of the general formula I to a form used as a fluorescent dye. The process including: a) dissolving or suspending the perylene-3,4:9,10-tetracarboximide in a solvent to obtain a solution or suspension; and b1) cooling the solution obtained in step a) to a temperature at or below the crystallization temperature of the perylene-3,4:9,10-tetracarboximide and, if the solvent is organic, removing excess solvent until the first crystals form, otherwise, adding water or dilute aqueous solutions of the solvent until the first crystals form, and maintaining the solution at that temperature for further crystallization; or b2) cooling the suspension obtained in step a) to or below the crystallization temperature when the temperature in step a) was above the crystallization temperature, and maintaining the suspension at the temperature for further crystallization to form one or more solvate crystals.

    摘要翻译： 将通式I的苝-3,4：9,10-四甲酰亚胺转化为用作荧光染料的形式的新型晶型和方法。 该方法包括：a）将苝-3,4：9,10-四甲酰亚胺溶解或悬浮在溶剂中以获得溶液或悬浮液; 和b1）将步骤a）中获得的溶液冷却至等于或低于苝-3,4:9,10-四甲酰亚胺的结晶温度的温度，如果溶剂是有机的，则除去多余的溶剂直到形成第一晶体， 否则，加入水或稀释的溶剂水溶液直到形成第一晶体，并将溶液保持在该温度下进一步结晶; 或b2）当步骤a）中的温度高于结晶温度时，将步骤a）中获得的悬浮液冷却至或低于结晶温度，并将悬浮液保持在该温度下进一步结晶以形成一种或多种溶剂化物晶体。

    Method for the production of perylen-3,4:9,10-tetracarboxylic acid diimides and perylen-3,4:9,10-tetracarboxylic acid dianhydride and naphtalene-1,8-dicarboxylimides
    3.
    发明申请
    Method for the production of perylen-3,4:9,10-tetracarboxylic acid diimides and perylen-3,4:9,10-tetracarboxylic acid dianhydride and naphtalene-1,8-dicarboxylimides 有权

    公开(公告)号：US20050131220A1

    公开(公告)日：2005-06-16

    申请号：US10510579

    申请日：2003-04-15

    申请人： Bernhard Dung ,  Felix Muller ,  Arno Bohm ,  Willi Helfer ,  Volker Wevrauch ,  Georg Henning

    发明人： Bernhard Dung ,  Felix Muller ,  Arno Bohm ,  Willi Helfer ,  Volker Wevrauch ,  Georg Henning

    IPC分类号： C07D221/14 ,  C07D487/06 ,  C09B5/62 ,  C09B57/08 ,  C07D471/02

    CPC分类号： C09B5/62 ,  C09B57/08

    摘要： A process for preparing perylene-3,4:9,10-tetracarboxylic diimides of the general formula I where R is C1-C30-alkyl whose carbon chain may be interrupted by one or more —O— moieties and/or which may be substituted by one or more substituents selected from the group consisting of C5-C8-cycloalkyl (which may be substituted by one or more C1-C6-alkyl substituents), phenyl or phenyl-C1-C6-alkyl (which may each be substituted by one or more C1-C18-alkyl and/or C1-C6-alkoxy substituents), —OCOR1, —N(R1)2, —SO2NH2, —SO2N(R1)2, —CON(R1)2 and —COOR1; C5-C8-cycloalkyl whose carbon skeleton may be interrupted by one or more moieties selected from the group consisting of —O—, —S— and —NR2- and/or which may be substituted by one or more C1-C6-alkyl substituents; phenyl, phenyl-C1-C6-alkyl, naphthyl or hetaryl, which may each be substituted by one or more substituents selected from the group consisting of C1-C18-alkyl, C1-C6-alkoxy, phenylazo, naphthylazo, pyridylazo, pyrimidylazo, cyano, —N(R1)2, —CON(R1)2 and —COOR1; R1 is C1-C6-alkyl, C5-C8-cycloalkyl, phenyl or phenyl-C1-C6-alkyl; R2 is C1-C6-alkyl, phenyl or phenyl-C1-C6-alkyl, by dimerizing a naphthalene-1,8-dicarboximide of the formula II comprises effecting said dimerizing in a reaction medium consisting essentially of an a polar aprotic organic solvent and an alkali metal base and subsequently reoxidizing the resulting alkali metal salt of the leuco form of the perylene-3,4:9,10-tetracarboxylic diimide in the presence of a polar solvent, and also preparation of perylene-3,4:9,10-tetracarboxylic dianhydride and naphthalene-1,8-dicarboximides.

    Method for converting perylen-3,4:9,10-tetracarboxylic acid diimides into a form suitable for use as a fluorescent dye
    7.
    发明申请
    Method for converting perylen-3,4:9,10-tetracarboxylic acid diimides into a form suitable for use as a fluorescent dye 有权
    将苝-3,4：9,10-四羧酸二酰亚胺转化为适合用作荧光染料的形式的方法

    公开(公告)号：US20050251930A1

    公开(公告)日：2005-11-17

    申请号：US10514564

    申请日：2003-06-06

    申请人： Peter Erk ,  Simone Schafer ,  Arno Bohm ,  Peter Blaschka ,  Harald Arms ,  Willi Helfer

    发明人： Peter Erk ,  Simone Schafer ,  Arno Bohm ,  Peter Blaschka ,  Harald Arms ,  Willi Helfer

    IPC分类号： C09B67/10 ,  C09B67/48 ,  D06P3/52

    CPC分类号： C09B67/0014 ,  C09B67/0025

    摘要： A process for converting perylene-3,4:9,10-tetracarboximides of the general formula I in which R1 and R2 are each unbranched, branched or cyclic C1-C8-alkyl to a form suitable for use as fluorescent dyes, which comprises a) dissolving or suspending the perylene-3,4:9,10-tetracarboximides in an organic or inorganic solvent whose molecules have a molecular volume of ≦230 Å3 at from 0 to 250° C., b1) cooling the solution obtained in step a) to or below the crystallization temperature and, in the case of an organic solvent, if desired at the same time removing excess solvent until the first crystals form, or, in the case of an inorganic solvent, adding water or dilute aqueous solutions of the solvent until the first crystals form, and maintaining the solution at this temperature for further crystallization or b2) cooling the suspension obtained in step a) to or below the crystallization temperature when the temperature in step a) was above the crystallization temperature, and maintaining the suspension at this temperature for further crystallization, c) isolating the solvate crystals formed in step b) and d) then removing the solvent from the solvate crystals, and also novel crystalline forms of perylene-3,4:9,10-tetracarboxylic diimides.

    摘要翻译： 用于转化通式I的苝-3,4：9,10-四甲酰亚胺的方法，其中R 1和R 2各自为非支链，支链或环状C < SUB-1-C 8 - 烷基至适于用作荧光染料的形式，其包括：a）将苝-3,4：9,10-四甲酰亚胺溶解或悬浮于 分子在0-250℃下具有分子体积<= 230Å3的有机或无机溶剂，b1）将步骤a）中获得的溶液冷却至或低于结晶温度， 在有机溶剂的情况下，如果需要，同时除去过量的溶剂，直到形成第一晶体，或者在无机溶剂的情况下，加入水或溶剂的稀溶液直到形成第一晶体，并保持 在该温度下进一步结晶的溶液或b2）当步骤a）中的温度wa）时将步骤a）中得到的悬浮液冷却至或低于结晶温度 高于结晶温度，并将悬浮液保持在该温度下进一步结晶，c）分离步骤b）中形成的溶剂化物晶体，d）然后从溶剂合物晶体中除去溶剂，以及新型苝-3的结晶形式， 4：9,10-四羧酸二酰亚胺。

    Preparation of perylen-3,4:9,10-tetracarboxylic dianhydride and also of naphtalene-1,8-dicarboximides
    8.
    发明授权
    Preparation of perylen-3,4:9,10-tetracarboxylic dianhydride and also of naphtalene-1,8-dicarboximides 有权
    苝-3,4：9,10-四羧酸二酐以及萘-1,8-二羧酰亚胺的制备

    公开(公告)号：US07807836B2

    公开(公告)日：2010-10-05

    申请号：US11955605

    申请日：2007-12-13

    申请人： Bernhard Dung ,  Felix Mueller ,  Arno Boehm ,  Willi Helfer ,  Volker Weyrauch ,  Georg Henning

    发明人： Bernhard Dung ,  Felix Mueller ,  Arno Boehm ,  Willi Helfer ,  Volker Weyrauch ,  Georg Henning

    IPC分类号： C07D471/16 ,  C07D471/00

    CPC分类号： C09B5/62 ,  C09B57/08

    摘要： A process for preparing perylene-3,4:9,10-tetracarboxylic dianhydride, comprising: dimerizing a naphthalene-1,8-dicarboximide of the formula IIa; reoxidizing the resulting alkali metal salt of the leuco form of the perylene-3,4:9,10-tetracarboxylic diimide of the formula Ia; hydrolyzing the diimide to the tetraalkali metal salt of perylene-3,4:9,10-tetracarboxylic acid in the presence of an inert organic solvent, of an alkali metal base and of water; and subjecting the tetraalkali metal salt of perylene-3,4:9,10-tetracarboxylic acid to the action of an aqueous inorganic acid to convert it into perylene-3,4:9,10-tetracarboxylic dianhydride; wherein R3 is cyclohexyl or phenyl which may each be substituted by up to three C1-C4-alkyl radicals, and the dimerizing is in a substantially homogeneous reaction medium consisting essentially of an apolar aprotic organic solvent and an alkali metal base.

    摘要翻译： 一种制备苝-3,4：9,10-四羧酸二酐的方法，包括：使式IIa的萘-1,8-二甲酰亚胺二聚化; 重新氧化得到的无水形式的式Ia的苝-3,4：9,10-四羧酸二酰亚胺的碱金属盐; 在惰性有机溶剂，碱金属碱和水的存在下将二酰亚胺水解成苝-3,4：9,10-四羧酸的四碱金属盐; 并将苝-3,4：9,10-四羧酸的四碱金属盐作为无机酸水溶液的作用，将其转化成苝-3,4：9,10-四羧酸二酐; 其中R 3是可以被至多三个C 1 -C 4 - 烷基取代的环己基或苯基，二聚在基本上均匀的反应介质中，其基本上由非极性非质子有机溶剂和碱金属碱组成。

    METHOD FOR CONVERTING PERYLEN-3,4:9,10-TETRACARBOXYLIC ACID DIIMIDES INTO A FORM SUITABLE FOR USE AS A FLUORESCENT DYE
    9.
    发明申请
    METHOD FOR CONVERTING PERYLEN-3,4:9,10-TETRACARBOXYLIC ACID DIIMIDES INTO A FORM SUITABLE FOR USE AS A FLUORESCENT DYE 审中-公开
    将季戊四烯-3,4：9,10-四羧酸二异氰酸酯转化为适用于荧光染料的形式的方法

    公开(公告)号：US20100218321A1

    公开(公告)日：2010-09-02

    申请号：US12718512

    申请日：2010-03-05

    申请人： Peter Erk ,  Simone Schäfer ,  Arno Böhm ,  Peter Blaschka ,  Harald Arms ,  Willi Helfer

    发明人： Peter Erk ,  Simone Schäfer ,  Arno Böhm ,  Peter Blaschka ,  Harald Arms ,  Willi Helfer

    IPC分类号： C09B5/00 ,  D06P5/00

    CPC分类号： C09B67/0014 ,  C09B67/0025

    摘要： Novel crystalline forms of and a process for converting perylene-3, 4:9, 10-tetracarboximide of the general formula I to a form used as a fluorescent dye. The process including: a) dissolving or suspending the perylene-3, 4:9, 10-tetracarboximide in a solvent to obtain a solution or suspension; and b1) cooling the solution obtained in step a) to a temperature at or below the crystallization temperature of the perylene-3, 4:9, 10-tetracarboximide and, if the solvent is organic, removing excess solvent until the first crystals form, otherwise, adding water or dilute aqueous solutions of the solvent until the first crystals form, and maintaining the solution at that temperature for further crystallization; or b2) cooling the suspension obtained in step a) to or below the crystallization temperature when the temperature in step a) was above the crystallization temperature, and maintaining the suspension at the temperature for further crystallization to form one or more solvate crystals.

    摘要翻译： 将通式I的苝-3,4：9,10-四甲酰亚胺转化成用作荧光染料的形式的新型结晶形式和方法。 该方法包括：a）将苝-3,4：9,10-四甲酰亚胺溶解或悬浮在溶剂中以获得溶液或悬浮液; 和b1）将步骤a）中获得的溶液冷却至等于或低于苝-3,4:9,10-四甲酰亚胺的结晶温度的温度，如果溶剂是有机的，则除去多余的溶剂直到形成第一晶体， 否则，加入水或稀释的溶剂水溶液直到形成第一晶体，并将溶液保持在该温度下进一步结晶; 或b2）当步骤a）中的温度高于结晶温度时，将步骤a）中获得的悬浮液冷却至或低于结晶温度，并将悬浮液保持在该温度下进一步结晶以形成一种或多种溶剂化物晶体。