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    Preparation of di-cation ethers
    3.
    发明授权
    Preparation of di-cation ethers 失效
    制剂的制备

    公开(公告)号：US5110937A

    公开(公告)日：1992-05-05

    申请号：US400844

    申请日：1989-08-30

    申请人： Derek D. Chapman ,  Ronald R. Valente

    发明人： Derek D. Chapman ,  Ronald R. Valente

    IPC分类号： C07D213/89 ,  C07D213/20 ,  C07D213/64

    CPC分类号： C07D213/64

    摘要： Di-cation ether salts are prepared by a reaction sequence which comprises(i) N-alkylating a 2-halopyridine,(ii) reacting the N-alkylated product with a 2-hydroxypyridine in the presence of sufficient organic base to combine with the by-product hydrohalic acid, and(iii) reacting the mono-cation ether thereby produced with an alkylating agent.The process is conducted in the presence of a solvent, such as acetonitrile. The di-cation can be isolated by removal of the solvent, followed by contacting the reaction mixture with an aqueous fluoborate, whereby the di-cation ether precipitates as the fluoborate salt. The di-cation ether is prepared in surprisingly high yield. The process can be conducted in one reaction vessel without isolation of a product intermediate formed in the reaction sequence. The fluoborate product is quite pure. If desired, the fluoborate anion can be removed from the di-cation ether by suspending the di-cation ether fluoborate in water, and reacting it with a potassium salt such as KNO.sub.3. The soluble di-cation product thereby produced can be used as a gelatin hardener, or as a chemical intermediate.

    摘要翻译： 二阳离子醚盐通过反应顺序制备，该反应顺序包括（i）N-烷基化2-卤代吡啶，（ii）在足够的有机碱的存在下使N-烷基化产物与2-羟基吡啶反应，与 - 产物氢卤酸，和（iii）使由此产生的单阳离子醚与烷基化剂反应。 该方法在溶剂如乙腈存在下进行。 可以通过除去溶剂来分离二阳离子，然后使反应混合物与氟硼酸盐接触，由此二阳离子醚作为氟硼酸盐沉淀。 二阳离子醚以惊人的高产率制备。 该方法可以在一个反应​​容器中进行，而不分离在反应顺序中形成的产物中间体。 氟硼酸盐产品是相当纯净的。 如果需要，可以通过将氟硼酸二阳离子醚悬浮在水中并将其与钾盐如KNO 3反应从二阳离子醚中除去氟硼酸根阴离子。 由此生产的可溶性二阳离子产物可以用作明胶硬化剂或作为化学中间体。

    One-pot synthesis of pyrazolotriazole photographic dye forming color couplers and coupler intermediates
    4.
    发明授权
    One-pot synthesis of pyrazolotriazole photographic dye forming color couplers and coupler intermediates 失效

    公开(公告)号：US6008369A

    公开(公告)日：1999-12-28

    申请号：US313011

    申请日：1999-05-17

    申请人： Ronald R. Valente ,  Judith A. Bose

    发明人： Ronald R. Valente ,  Judith A. Bose

    IPC分类号： C07D487/04 ,  G03C7/38

    CPC分类号： C07D487/04

    摘要： Photographic pyrazolotriazole dye forming coupler compounds of coupler intermediate compounds can be readily prepared in a single reaction medium by reacting certain pyrazolotriazole compounds with nitro-substituted aromatic compounds in the presence of a formate salt and a transition metal catalyst. This salt hydrogenates the nitro group and the carbonate by-product induces reaction of the resulting amine with the pyrazolotriazole compound. Yields and purity are high, and reaction time is reduced with the specific set of conditions and reactants, and environmental impact from waste is reduced. In addition, isolation of aromatic amine intermediates is avoided. The resulting pyrazolotriazole compounds can be used themselves as photographic dye forming couplers or further reacted to prepare useful coupler compounds for photographic use.

    Aldophosphamide derivatives useful as antitumor agents
    6.
    发明授权
    Aldophosphamide derivatives useful as antitumor agents 失效
    可用作抗肿瘤剂的二磷酰胺衍生物

    公开(公告)号：US4908356A

    公开(公告)日：1990-03-13

    申请号：US198429

    申请日：1988-05-25

    申请人： Richard F. Borch ,  Ronald R. Valente

    发明人： Richard F. Borch ,  Ronald R. Valente

    IPC分类号： C07F9/6533 ,  C07F9/6558

    CPC分类号： C07F9/65583 ,  C07F9/6533

    摘要： A compound of the formula ##STR1## wherein R.sup.1 and R.sup.2 may be the same of different and are each independently hydrogen or lower alkyl which may be unsubstituted or monosubstituted with halogen, lower alkoxy or hydroxy with the proviso that the substituent is not the .alpha.-carbon or R.sup.1 and R.sup.2 taken together with the carbon to which they are attached form a morpholino ring;each R.sup.3 is independently hydrogen, lower alkyl, carboxy or carbalkoxy;n is an integer from 0, 1, 2 or 3 andR is hydrogen, lower alkyl, cycloalkyl, arylalkyl aryl or a nitrogen, sulfur or oxygen containing heterocyclic or a heterocyclic lower alkyl and pharmacuetically acceptable salts thereof.

    摘要翻译： 式IMA的化合物，其中R 1和R 2可以是不同的且各自独立地是氢或可以被未取代的或被卤素，低级烷氧基或羟基单取代的低级烷基，条件是取代基不是α- 碳或R1和R2与它们所连接的碳一起形成吗啉环; 每个R 3独立地为氢，低级烷基，羧基或烷氧羰基; n为0,1,2或3的整数，R为氢，低级烷基，环烷基，芳基烷基芳基或含氮，硫或含氧杂环或杂环低级烷基及其药理学上可接受的盐。

    Synthesis of pyrazolotriazole photographic dye forming color couplers and intermediates
    7.
    发明授权
    Synthesis of pyrazolotriazole photographic dye forming color couplers and intermediates 失效
    吡唑并三唑照相染料的合成形成色成色剂和中间体

    公开(公告)号：US5998629A

    公开(公告)日：1999-12-07

    申请号：US204444

    申请日：1998-12-02

    申请人： Judith A. Bose ,  Ronald R. Valente ,  Dino Aimino ,  Deborah D. DeMejo

    发明人： Judith A. Bose ,  Ronald R. Valente ,  Dino Aimino ,  Deborah D. DeMejo

    IPC分类号： C07D487/04 ,  G03C7/38 ,  C07D249/18

    CPC分类号： C07D487/04 ,  G03C7/3835

    摘要： Photographic pyrazolotriazole dye forming coupler compound or coupler intermediate compounds can be readily prepared by inducing an elimination-addition reaction between certain pyrazolotriazole compounds and aromatic amines in the presence of an inorganic base or formate. Yields and purity are high, and reaction time is reduced with the specific set of conditions and reactants, and environmental impact from waste is reduced. The resulting compounds can be used themselves as photographic dye forming couplers or further reacted to prepare useful coupler compounds for photographic use.

    摘要翻译： 通过在无机碱或甲酸盐的存在下，通过诱导某些吡唑并三唑化合物和芳族胺之间的消除加成反应，可容易地制备形成吡唑并三唑染料的成色剂化合物或成色剂中间体化合物。 产量和纯度高，反应时间随特定条件和反应物的降低而减少，浪费对环境的影响降低。 所得化合物可以自身用作照相染料形成成色剂或进一步反应以制备用于照相用途的有用的成色剂化合物。

    Photographic element containing an improved pyrozolotriazole coupler
    8.
    发明授权
    Photographic element containing an improved pyrozolotriazole coupler 失效
    含有改进的焦唑三唑成色剂的摄影元件

    公开(公告)号：US5985532A

    公开(公告)日：1999-11-16

    申请号：US725726

    申请日：1996-10-04

    申请人： Judith A. Bose ,  Louis E. Friedrich ,  David Hoke ,  Joan C. Potenza ,  Robert F. Romanet ,  Stephen P. Singer ,  Ronald R. Valente

    发明人： Judith A. Bose ,  Louis E. Friedrich ,  David Hoke ,  Joan C. Potenza ,  Robert F. Romanet ,  Stephen P. Singer ,  Ronald R. Valente

    IPC分类号： G03C7/00 ,  C07D487/04 ,  G03C7/32 ,  G03C7/38 ,  G03C1/08 ,  G03C7/26

    CPC分类号： C07D487/04 ,  G03C7/3835 ,  G03C7/3212

    摘要： The invention provides a photographic element comprising a light sensitive silver halide emulsion layer having associated therewith a dye-forming coupler having formula I: ##STR1## wherein R.sub.1 is selected from the group consisting of alkyl, aryl, and heterocyclic groups;R.sub.2 is selected from the group consisting of hydrogen, alkyl, aryl, and heterocyclic groups;W is C(O) or S(O).sub.2 ;R.sub.3 is selected from the group consisting of alkyl, alkoxy, aryl, aryloxy, and amino groups;each R.sub.4 is independently selected from the group consisting of alkyl, alkoxy, aryl, aryloxy, and alkylamino groups, and n is an integer from 1 to 4;Y is a substituent; andX is H or a coupling-off group;provided that the number of carbon atoms contained in R.sub.1, R.sub.2, R.sub.3 and R.sub.4 combined is at least 18 and provided further that any two or more of R.sub.1, R.sub.2, R.sub.3 and R.sub.4 may be joined to form a ring.

    摘要翻译： 本发明提供了一种照相元件，其包含光敏卤化银乳剂层，其具有式I的染料形成成色剂：其中R1选自烷基，芳基和杂环基; R2选自氢，烷基，芳基和杂环基; W是C（O）或S（O）2; R3选自烷基，烷氧基，芳基，芳氧基和氨基; 每个R 4独立地选自烷基，烷氧基，芳基，芳氧基和烷基氨基，n是1至4的整数; Y是取代基; X为H或偶合离去基团; 条件是R 1，R 2，R 3和R 4中所含的碳原子数目至少为18，并且进一步提供R 1，R 2，R 3和R 4中的任何两个或更多个可以连接形成环。

    One-pot synthesis of pyrazolotriazole photographic dye forming color couplers and coupler intermediates
    9.
    发明授权
    One-pot synthesis of pyrazolotriazole photographic dye forming color couplers and coupler intermediates 失效
    吡啶三唑照相染料的一锅合成形成色耦合剂和偶联剂中间体

    公开(公告)号：US5969148A

    公开(公告)日：1999-10-19

    申请号：US203459

    申请日：1998-12-02

    申请人： Ronald R. Valente ,  Judith A. Bose

    发明人： Ronald R. Valente ,  Judith A. Bose

    IPC分类号： C07D487/04 ,  G03C7/38

    CPC分类号： C07D487/04

    摘要： Photographic pyrazolotriazole dye forming coupler compounds of coupler intermediate compounds can be readily prepared in a single reaction medium by reacting certain pyrazolotriazole compounds with nitro-substituted aromatic compounds in the presence of a formate salt and a transition metal catalyst. This salt hydrogenates the nitro group and the carbonate by-product induces reaction of the resulting amine with the pyrazolotriazole compound. Yields and purity are high, and reaction time is reduced with the specific set of conditions and reactants, and environmental impact from waste is reduced. In addition, isolation of aromatic amine intermediates is avoided. The resulting pyrazolotriazole compounds can be used themselves as photographic dye forming couplers or further reacted to prepare useful coupler compounds for photographic use.

    摘要翻译： 通过在甲酸盐和过渡金属催化剂的存在下使某些吡唑并三唑化合物与硝基取代的芳族化合物反应，可以在单一反应介质中容易地制备成色剂中间体化合物的成像吡唑并三唑染料形成成色剂化合物。 该盐使硝基氢化，碳酸酯副产物诱导所得胺与吡唑并三唑化合物的反应。 产量和纯度高，反应时间随特定条件和反应物的降低而减少，浪费对环境的影响降低。 此外，避免了芳族胺中间体的分离。 所得的吡唑并三唑化合物可以自己用作成像成色剂的照相染料，或进一步反应以制备用于照相用途的有用的成色剂化合物。