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    Nitrophenyl imino propionates
    1.
    发明授权
    Nitrophenyl imino propionates 失效
    硝基苯基亚氨基丙酸酯

    公开(公告)号：US4138571A

    公开(公告)日：1979-02-06

    申请号：US742011

    申请日：1976-11-15

    申请人： David J. Tracy ,  Walter F. Hoffstadt

    发明人： David J. Tracy ,  Walter F. Hoffstadt

    IPC分类号： C07C119/20

    CPC分类号： C07D209/08

    摘要： A feature of the present invention is the provision of imidic esters having halo and nitro substituents on the phenyl ring attached to the nitrogen atom of the imidic ester, and of a method for preparing such compounds in high yields. In accordance with the process of the present invention, it has been found that imidic esters can be prepared in high yields using available starting materials. In the process, an alkyl .beta.-alkoxy-.beta.-iminopropionate salt is reacted first with a suitable alkanol to form an orthoester intermediate in situ. Then the orthoester is converted in high yields to the corresponding imidic ester by condensation with an aniline while simultaneously removing alkanol from the reaction mixture to drive the equilibrium reaction to completion. In a preferred form of the invention, the formation of the imidic ester is carried out in a high boiling solvent whose presence enables the condensation to be carried out more effectively at a high temperatue than with alkanol alone. Particularly, the high boiling solvent mixture adds volume to the reaction mixture which enables good agitation of the reactants at a predetermined and measureable reaction temperature. Furthermore, it facilitates the simultaneous distillation of the more volatile alkanol by-product from the reaction mixture.

    摘要翻译： 本发明的一个特征是提供在与酰亚胺酯的氮原子连接的苯环上具有卤代和硝基取代基的酰亚胺酯，以及高产率制备这些化合物的方法。 根据本发明的方法，已经发现可以使用可用的起始原料以高收率制备亚胺酯。 在此过程中，β-烷氧基-β-亚氨基丙酸烷基酯盐首先与合适的链烷醇反应以原位形成原酸酯中间体。 然后通过与苯胺缩合，将原酸酯以高收率转化成相应的酰亚胺酯，同时从反应混合物中除去链烷醇以促使平衡反应完成。 在本发明的优选形式中，酰亚胺酯的形成在高沸点溶剂中进行，其存在使得能够在高温下比单独使用链烷醇更有效地进行缩合。 特别地，高沸点溶剂混合物增加了反应混合物的体积，这使得能够在预定和可测量的反应温度下良好地搅拌反应物。 此外，它有助于从反应混合物中同时蒸馏更易挥发的链烷醇副产物。

    Process for the preparation of 3-anilino-5-pyrazolones
    3.
    发明授权
    Process for the preparation of 3-anilino-5-pyrazolones 失效
    制备3-苯胺基-5-吡唑啉酮的方法

    公开(公告)号：US4113954A

    公开(公告)日：1978-09-12

    申请号：US742058

    申请日：1976-11-15

    申请人： David J. Tracy ,  Walter F. Hoffstadt

    发明人： David J. Tracy ,  Walter F. Hoffstadt

    IPC分类号： G03C7/38 ,  C07C67/00 ,  C07C239/00 ,  C07C241/00 ,  C07C257/04 ,  C07C257/14 ,  C07D231/22 ,  C07D231/52 ,  C09B55/00 ,  G03C7/384

    CPC分类号： C07C251/72 ,  C07D231/52 ,  G03C7/384

    摘要： In accordance with the present invention, it has been found that 3-anilino-5-pyrazolones can be prepared in high yields by a multi-step process using available starting materials. In the first step of the process, an alkyl .beta.-alkoxy-.beta.-iminopropionate salt is reacted with a suitable alkanol to form an orthoester intermediate in situ. The orthoester then is converted in high yields to the corresponding imidic ester by condensation with an aniline while simultaneously removing alkanol from the reaction mixture to drive the equilibrium reaction to completion. In a preferred form of the invention, formation of the imidic ester is carried out in a high boiling solvent whose presence enables the condensation to be carried out effectively at a high temperature, and which facilitates distillation of the more volatile alkanol by-product from the reaction mixture at atmospheric pressure.

    摘要翻译： 本发明的脒化合物具有以下通式：其中R 2为低级烷基，R为被卤素和硝基取代的苯基，R 3选自苯基和被一个或多个卤素，硝基和烷氧基取代的苯基，以及 其组合可有利地用作制造特别有用的高质量吡唑啉酮成色剂的中间体，其通过本领域已知的其它方法或技术证明特别难以高产率制备。

    Process for the preparation of high purity imidazoline based amphoacetate surfactants
    8.
    发明授权
    Process for the preparation of high purity imidazoline based amphoacetate surfactants 失效
    制备高纯度咪唑啉基二乙酸酯表面活性剂的方法

    公开(公告)号：US5952291A

    公开(公告)日：1999-09-14

    申请号：US55368

    申请日：1998-04-06

    申请人： Bharat Desai ,  Peter Lees ,  Jean-Marc Ricca ,  David J. Tracy

    发明人： Bharat Desai ,  Peter Lees ,  Jean-Marc Ricca ,  David J. Tracy

    IPC分类号： A61K8/00 ,  A61K8/40 ,  A61K8/44 ,  A61K8/49 ,  A61Q5/00 ,  A61Q5/02 ,  A61Q19/10 ,  B01F17/00 ,  B01F17/16 ,  B01F17/22 ,  B01F17/28 ,  C07C233/36 ,  C07C233/38 ,  C07D233/02 ,  C07D233/04 ,  C07D233/14 ,  C11D1/40 ,  C11D1/88 ,  C11D3/43 ,  C11D7/32 ,  C11D7/50 ,  B01F17/32

    CPC分类号： C11D7/5022 ,  A61K8/442 ,  A61K8/4946 ,  A61Q19/10 ,  A61Q5/02 ,  B01F17/0042 ,  B01F17/0085 ,  C07C233/36 ,  C07C233/38 ,  C07D233/02 ,  C11D1/40 ,  C11D1/88 ,  C11D3/43 ,  C11D7/3209 ,  C11D7/3218 ,  C11D7/5013 ,  C11D7/5018 ,  Y10S516/915

    摘要： Imadazoline-based amphoacetates of higher purity, containing essentially negligible amounts of unalkylated amido amines, lower amounts of glycolic acid salts and monochloroacetate salts, superior to currently available conventional amphoacetates, are provided. This is demonstrated by their improved surface-active properties. Lower inherent irritation properties may be expected due to improved purity.The higher purity amphoacetates can be obtained via processes utilizing precise pH control during the reaction of imidazoline, or its open-chain derivatives, with alkylating agents, e.g. sodium monochloroacetate. The pH can be controlled by adding the base slowly or automatically in response to a pH metering device to maintain a constant pH, or by a series of staged additions which are calculated to maintain pH within a stated range. The reaction may also be carried out by conducting the initial hydrolysis of the imidazoline ring structure, followed by alkylation. These higher-purity amphoacetates contain essentially fully alkylated products and lower amounts of glycolic acid derivatives, even though a ratio of SMCA to substituted imidazoline, or its open-ring derivative, of less than 1.5:1.0 and close to 1.0:1.0 is used.

    摘要翻译： 提供了更高纯度的基于咪达唑啉的两性乙酸盐，其含有基本上可忽略量的未烷基化的酰胺胺，较低量的乙醇酸盐和一氯乙酸盐，优于现有常规的两性乙酸盐。 这通过其改进的表面活性特性证明。 由于纯度的提高，预期会降低固有的刺激性能。 可以通过在咪唑啉或其开链衍生物与烷基化试剂反应期间利用精确的pH控制的方法获得较高纯度的两性乙酸酯，例如。 一氯乙酸钠。 可以通过缓慢或自动地加入碱来控制pH，以响应于pH计量装置以保持恒定的pH，或通过一系列分级添加剂来计算，以将pH保持在规定范围内。 该反应也可以通过进行咪唑啉环结构的初始水解，然后进行烷基化来进行。 尽管SMCA与取代的咪唑啉或其开环衍生物的比例小于1.5：1.0且接近1.0：1.0，但这些较高纯度的两性乙酸盐基本上含有完全烷基化产物和较少量的乙醇酸衍生物。