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    • 4. 发明授权
    • One-pot synthesis of pyrazolotriazole photographic dye forming color
couplers and coupler intermediates
    • 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
    • US5969148A
    • 1999-10-19
    • US203459
    • 1998-12-02
    • Ronald R. ValenteJudith A. Bose
    • Ronald R. ValenteJudith A. Bose
    • C07D487/04G03C7/38
    • C07D487/04
    • 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.
    • 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。
    • 6. 发明授权
    • Preparation of di-cation ethers
    • 制剂的制备
    • US5110937A
    • 1992-05-05
    • US400844
    • 1989-08-30
    • Derek D. ChapmanRonald R. Valente
    • Derek D. ChapmanRonald R. Valente
    • C07D213/89C07D213/20C07D213/64
    • C07D213/64
    • 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.
    • 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。