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    Aqueous liquid composition of fluorescent brightener excellent in dyeing characteristics
    3.
    发明申请
    Aqueous liquid composition of fluorescent brightener excellent in dyeing characteristics 失效
    荧光增白剂的水性液体组合物的染色特性优异

    公开(公告)号：US20040111812A1

    公开(公告)日：2004-06-17

    申请号：US10472322

    申请日：2003-09-18

    Inventor： Toru Yamaguchi ,  Nobutaka Yamamoto

    IPC: C09B001/00

    CPC classification number: C09B47/18 ,  C07D251/68 ,  C07D251/70 ,  D06L4/621 ,  D06P1/0012 ,  D21H21/30 ,  Y10S8/919

    Abstract: An aqueous liquid composition characterized by containing an alkali salt, an alkali metal salt, an alkali earth metal salt or an ammonium salt of a compound represented by the following formula (1). 1 in the form of free acid in an amount of 10-40 mass % and inorganic salt in an amount of 1.1-10 mass % can easily be produced without a desalting process or the like which has been included in a conventional process and it has an excellent storage stability and excellent fluorescent brightening effect.

    Abstract translation: 一种含水液体组合物，其特征在于含有下式（1）表示的化合物的碱金属盐，碱金属盐，碱土金属盐或铵盐。 以10〜40质量％的游离酸的形式，以及1-10质量％的无机盐可以容易地制备，而不需要在常规方法中包括的脱盐方法等，并且其具有 优良的储存稳定性和优异的荧光增白效果。

    Process for the preparation of stilbene compounds
    4.
    发明授权
    Process for the preparation of stilbene compounds 失效
    二苯乙烯化合物的制备方法

    公开(公告)号：US06365737B1

    公开(公告)日：2002-04-02

    申请号：US09622472

    申请日：2000-08-17

    Applicant: Georges Metzger ,  Fabienne Cuesta ,  Peter Rohringer ,  Dieter Reinehr ,  René Schlatter

    Inventor： Georges Metzger ,  Fabienne Cuesta ,  Peter Rohringer ,  Dieter Reinehr ,  René Schlatter

    IPC: C07D25168

    CPC classification number: C11D3/42 ,  C07D251/68 ,  D06L4/621 ,  D06M2200/25 ,  D21H21/30

    Abstract: A process for the preparation of a 4,4′-bis-(triazinylamino)-stilbene-2,2′-disulphonic acid compound of formula (1) is disclosed, characterized in that (a) in a first reaction step cyanurchloride is reacted with the disodium salt of 4,4′-diaminostilbene-2,2′-disulfonic acid to give the intermediate of formula (2); (b) in a second reaction step the compound of formula (2) is reacted with a compound of formula R1—H and/or R2—H to give the compound of formula (3); (c) in a third step the compound of formula (3) is reacted with the compound of the formula R3H, and reaction step (a) and/or (c) are carried out in a medium consisting of a mixture of water and a polyglycol to give the compound of formula (1), wherein R1, R2 and R3, independently, are phenylamino; phenylamino substitued by C1-C3alkyl, halogen, cyano, COOR or COR; CONH—R; SO2NH—R; NH—COR; mono- or disulphonated phenylamino; morpholino; piperidino; pyrrolidino; —NH2; —NH(C1-C4alkyl); —N(C1-C4alkyl)2; —NH(C2-C4hydroxyalkyl); —N(C2-C4hydroxyalkyl)2; —N(C1-C4alkyl)(C2-C4hydroxyalkyl); NHC2-C4 alkylsulphonic acid; —OC1-C4alkyl; an aminoacid or aminoacid amide residue from which a hydrogen atom on the amino group has been removed; R1 and R2 may further independently represent hydrogen; C1-C4alkyl; phenyl; naphthyl; phenyl or naphthyl substituted by C1-C4alkyl, C1-C4alkoxy, halogen, C2-C5alkanoyl-amino, nitro, sulpho or C1-C4alkylated amino; R is hydrogen; or C1-C3alkyl; and M is H, Na, Li, K, Ca, Mg, ammonium, or ammonium that is mono-, di-, tri- or tetrasubstituted by C1-C4alkyl, C2-C4hydroxyalkyl or a mixture thereof.

    Abstract translation: 公开了制备式（1）的4​​,4'-双 - （三嗪基氨基） - 茋-2,2'-二磺酸化合物的方法，其特征在于（a）在第一反应步骤中，氰化氢反应 与4,4'-二氨基芪-2,2'-二磺酸的二钠盐得到式（2）的中间体; （b）在第二反应步骤中，将式（2）化合物与式R 1 -H和/或R 2 -H的化合物反应，得到式（3）化合物; （c）在第三步中，式（3）化合物与式R3H的化合物反应，反应步骤（a）和/或（c）在由水和 得到式（1）化合物，其中R 1，R 2和R 3独立地是苯基氨基; 由C 1 -C 3烷基，卤素，氰基，COOR或COR取代的苯基氨基; CONH-R; SO2NH-R; NH-COR; 单或二磺基苯基氨基; 吗啉代 哌啶子 吡咯烷 -NH2; -NH（C 1 -C 4烷基）; -N（C 1 -C 4烷基）2; -NH（C 2 -C 4羟烷基）; -N（C 2 -C 4羟烷基）2; -N（C 1 -C 4烷基）（C 2 -C 4羟烷基）; NHC2-C4烷基磺酸; -OC1-C4烷基; 已除去氨基上的氢原子的氨基酸或氨基酸酰胺残基; R 1和R 2可以进一步独立地表示氢; C 1 -C 4烷基; 苯基; 萘基; 被C 1 -C 4烷基，C 1 -C 4烷氧基，卤素，C 2 -C 5烷酰基 - 氨基，硝基，磺基或C 1 -C 4烷基化氨基取代的苯基或萘基; R是氢; 或C 1 -C 3烷基; 并且M是被C 1 -C 4烷基，C 2 -C 4羟烷基或其混合物单，二，三或四取代的H，Na，Li，K，Ca，Mg，铵或铵。

    Triazinylaminostilbene compounds
    5.
    发明授权
    Triazinylaminostilbene compounds 有权
    三嗪基氨基芪化合物

    公开(公告)号：US06331626B1

    公开(公告)日：2001-12-18

    申请号：US09666768

    申请日：2000-09-21

    Applicant: Peter Rohringer ,  André Geoffroy ,  Andreas Burkhard ,  Erwin Marti ,  Werner Schreiber ,  Josef Zelger

    Inventor： Peter Rohringer ,  André Geoffroy ,  Andreas Burkhard ,  Erwin Marti ,  Werner Schreiber ,  Josef Zelger

    IPC: C07D25170

    CPC classification number: C07D251/68 ,  C09B67/0025 ,  D06L4/621 ,  Y10S8/919

    Abstract: The present invention provides a hydrate of the 4,4′-di-triazinylamino-2,2′-di-sulfostilbene compound having the formula: in which M and M1 independently represent hydrogen, an alkaline-, an alkaline earth metal or ammonium, x is a number within the range of from 1 to 30, and the crystal form of the hydrate (I) being characterised by an X-ray diffraction pattern which is essentially as set out in the accompanying FIGS. 1 to 11; or a mixture containing one or more of the hydrates of the 4,4′-di-triazinylamino-2,2′-di-sulfostilbene compound having the formula (I); processes for the preparation of the new hydrates; and the use of the new hydrates for the preparation of concentrated aqueous formulations of fluorescent whitening agents.

    Abstract translation: 本发明提供了具有下式的4,4'-二 - 三嗪基氨基-2,2'-二磺基芪化合物的水合物：其中M和M1独立地表示氢，碱金属，碱土金属或铵， x是1至30范围内的数字，并且水合物（I）的晶体形式的特征在于X射线衍射图，其基本上如附图中所示。 1至11; 或含有一种或多种具有式（I）的4,4'-二 - 三嗪基氨基-2,2'-二磺基芪化合物的水合物的混合物; 新水合物的制备过程; 以及使用新的水合物来制备荧光增白剂的浓缩水性制剂。

    Fluorescent whitening agents
    6.
    发明申请
    Fluorescent whitening agents 失效
    荧光增白剂

    公开(公告)号：US20010014989A1

    公开(公告)日：2001-08-23

    申请号：US09766984

    申请日：2001-01-22

    Inventor： Peter Rohringer ,  Georges Metzger ,  Dieter Reinehr

    IPC: D06L001/00 ,  C09B001/00 ,  C11D009/42

    CPC classification number: C09B23/148 ,  C07D251/68 ,  C11D3/42 ,  D06L4/621 ,  D06L4/657 ,  D06L4/75 ,  D06M13/07 ,  D06M13/358 ,  D06P1/6426 ,  D21H21/30 ,  Y10S8/919

    Abstract: The present invention provides new compounds having the formula: 1 in which X is O or, preferably, NH; M is hydrogen, an alkali metal atom, ammonium or a cation formed from an amine; each R1, independently, is an aminoacid residue from which a hydrogen atom on the amino group has been removed; n is 1 or 2; and each R2, independently, is hydrogen, C1-C3alkyl, halogen, cyano, COOR in which R is hydrogen or C1-C3alkyl, CONH-R in which R has its previous significance, SO2NH-R in which R has its previous significance, NH-COR in which R has its previous significance, SO3M in which M has its previous significance or, when n is 1, R2 can also be CO-R3 in which R3 is C1-C3alkyl or phenyl; provided that those compounds are excluded in which a) X is NH, n is 1 and R2 is SO3M in which M has its previous significance; or b) X is NH, n is 2 and one R2 is SO3M in which M has its previous significance, and the other R2 is hydrogen, methyl or halogen; or c) X is NH, n is 1, R1 is glycine and R2 is H or CO2H; or d) X is NH, n is 2, each R2 is SO3M in which M has its previous significance and the SO3M groups are in 2,5-positions in the phenyl ring and R1 is D,L-alanine, L-valine, L-leucine, L-isoleucine, L-threonine, L-aspartic acid, L-glutamic acid, L-phenylalanine, L-proline, (),L- methionine or glycine. Most of the new class of 4,4null-diaminostilbene-2,2null-disulfonic acid compounds are useful as fluorescent whitening agents, especially for paper.

    Abstract translation: 本发明提供了新的具有下式的化合物：其中X为O或优选为NH; M是氢，碱金属原子，铵或由胺形成的阳离子; 每个R 1独立地是氨基酸被除去的氨基酸残基; n为1或2; 并且每个R 2独立地是氢，C 1 -C 3烷基，卤素，氰基，其中R是氢或C 1 -C 3烷基的COOR，其中R具有其先前含义的CONH-R，其中R具有其先前含义的SO 2 NH- 其中R具有其先前含义的NH-COR，其中M具有其先前含义的SO 3 M，或当n为1时，R 2也可以是其中R 3为C 1 -C 3烷基或苯基的CO-R 3; 条件是排除这些化合物，其中a）X是NH，n是1，R2是其中M具有其先前意义的SO 3 M; 或b）X是NH，n是2，一个R2是SO3M，其中M具有其先前的含义，另一个R 2是氢，甲基或卤素; 或c）X是NH，n是1，R1是甘氨酸，R2是H或CO2H; 或d）X是NH，n是2，每个R2是SO3M，其中M具有其先前的意义，SO 3 M基团在苯环中是2.5位，R 1是D，L-丙氨酸，L-缬氨酸， L-亮氨酸，L-异亮氨酸，L-苏氨酸，L-天冬氨酸，L-谷氨酸，L-苯丙氨酸，L-脯氨酸，（），L-甲硫氨酸或甘氨酸。 大多数新类的4,4'-二氨基芪-2,2'-二磺酸化合物可用作荧光增白剂，特别是用于纸。

    Process for the preparation of sulphonated distyryl-biphenyl compounds
    7.
    发明授权
    Process for the preparation of sulphonated distyryl-biphenyl compounds 失效
    制备磺化二苯乙烯基 - 联苯化合物的方法

    公开(公告)号：US06274761B1

    公开(公告)日：2001-08-14

    申请号：US09646397

    申请日：2000-09-15

    Applicant: Victor Paul Eliu ,  Julia Völkel ,  Peter Rohringer ,  Roger Wolfgang Basler ,  Brigitte Gerhild Sereinig

    Inventor： Victor Paul Eliu ,  Julia Völkel ,  Peter Rohringer ,  Roger Wolfgang Basler ,  Brigitte Gerhild Sereinig

    IPC: C07C30300

    CPC classification number: C07C309/32 ,  C07C303/32 ,  C11D3/42 ,  D06L4/621 ,  D21H21/30

    Abstract: A process for the preparation of sulphonated distyryl-biphenyl compounds of formula (1), in which R1 and R2, independently, are hydrogen, C1-C5-alkyl, C1-C5-alkyl or halogen, and M represents Li, K, an alkaline earth metal or ammonium, characterized by, firstly, reacting a compound of formula (2) with a di- or trialkylamine containing 6-12 carbon atoms in each alkyl group, in a two-phase system consisting of strong aqueous mineral acid and a water immisicible organic solvent and, secondly, reacting the resulting lypophilic ammonium salt with LiOH, KOH, an alkaline earth metal hydroxide, ammonia, a mono-, di- or trialkylamine or a tetraalkylammonium hydroxide, all containing 1-4 carbon atoms in each alkyl group; mono-, di- or tri(C2-C4)alkanolamine, morpholine, piperdine or pyrrolidine.

    Abstract translation: 制备式（1）的磺化二苯乙烯基联苯化合物的方法，其中R 1和R 2独立地是氢，C 1 -C 5 - 烷基，C 1 -C 5 - 烷基或卤素，M代表Li，K， 碱土金属或铵，其特征在于：首先使式（2）化合物与每个烷基中含有6-12个碳原子的二 - 或三烷基胺反应，在由强无机酸和 水不溶性有机溶剂，其次，将所得的溶胞铵盐与LiOH，KOH，碱土金属氢氧化物，氨，一烷基，二或三烷基胺或四烷基氢氧化铵反应，其中每个烷基中都含有1-4个碳原子 组; 一，二或三（C 2 -C 4）链烷醇胺，吗啉，哌啶或吡咯烷。

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