公开(公告)号：US20090176985A1

公开(公告)日：2009-07-09

申请号：US12346262

申请日：2008-12-30

申请人： Peter ERK ,  Simone Schaefer ,  Arno Bohm ,  Peter Blaschka ,  Harald Arms ,  Willi Helfer

发明人： Peter ERK ,  Simone Schaefer ,  Arno Bohm ,  Peter Blaschka ,  Harald Arms ,  Willi Helfer

IPC分类号： C07D471/06

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0-250℃下将分子体积分数为<= 230的二萘嵌苯-3,4：9,10-四甲酰亚胺溶解或悬浮在有机或无机溶剂中，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 溶剂直至形成第一晶体，并将溶液保持在该温度下进一步结晶，或b）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，并维持 g在该温度下的悬浮液进一步结晶，c）分离步骤b）中形成的溶剂合物晶体，d）然后从溶剂合物晶体中除去溶剂，以及新型的苝-3,4：9,10-四羧酸的结晶形式 二酰亚胺

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

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。