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    Substituted 1,1,1-triaryl-2,2,2-trifluoroethanes and processes for their synthesis
    61.
    发明授权
    Substituted 1,1,1-triaryl-2,2,2-trifluoroethanes and processes for their synthesis 失效
    取代的1,1,1-三芳基-2,2,2-三氟乙烷及其合成方法

    公开(公告)号：US5011955A

    公开(公告)日：1991-04-30

    申请号：US419554

    申请日：1989-10-10

    Applicant: William B. Alston ,  Roy F. Gratz

    Inventor： William B. Alston ,  Roy F. Gratz

    IPC: C07C17/26 ,  C07C49/813 ,  C07C205/57 ,  C07F9/50

    CPC classification number: C07F9/5022 ,  C07C17/2637 ,  C07C201/14 ,  C07C209/78 ,  C07C51/367

    Abstract: Synthetic procedures to tetraalkyls, tetraacids and dianhydrides substituted 1,1,1-triaryl-2,2,2-trifluoroethanes which comprises: (1) 1,1-bis(dialkylaryl)-1-aryl-2,2,2-trifluoroethane, (2) 1,1-bis(dicarboxyaryl)-1-aryl-2,2,2-trifluoroethane or (3) cyclic dianhydride or diamine of 1,1-bis(dialkylaryl)-1-aryl-2,2,2-trifluoroethanes. The synthesis of (1) is accomplished by the condensation reaction of an aryltrifluoromethyl ketone with a dialkylaryl compound. The synthesis of (2) is accomplished by oxidation of (1). The synthesis dianhydride of (3) is accomplished by the conversion of (2) to its corresponding cyclic dianhydride. The synthesis of the diamine is accomplished by the similar reaction of an aryltrifluoromethyl ketone with aniline or alkyl substituted or disubstituted anilines. Also, other derivatives of the above are formed by nucleophilic displacement reactions.

    Abstract translation: 四烷基，四酸和二酐的合成方法取代1,1,1-三芳基-2,2,2-三氟乙烷，其包括：（1）1,1-双（二烷基芳基）-1-芳基-2,2,2-三氟乙烷 ，（2）1,1-双（二羧基芳基）-1-芳基-2,2,2-三氟乙烷或（3）1,1-双（二烷基芳基）-1-芳基-2,2,2-三氟乙烷的环状二酐或二胺， 2-三氟乙烷。 （1）的合成通过芳基三氟甲基酮与二烷基芳基化合物的缩合反应来实现。 （2）的合成通过（1）的氧化实现。 （3）的合成二酐通过（2）转化成其相应的环状二酐来实现。 二胺的合成通过芳基三氟甲基酮与苯胺或烷基取代或二取代的苯胺的类似反应来实现。 此外，上述的其它衍生物通过亲核取代反应形成。

    Cyclic two-stage nitration process for preparing 4-chloro-3,5-dinitrobenzotrifluoride from 4-chlorobenzotrifluoride
    63.
    发明授权
    Cyclic two-stage nitration process for preparing 4-chloro-3,5-dinitrobenzotrifluoride from 4-chlorobenzotrifluoride 失效
    从4-氯三氟甲苯制备4-氯-3,5-二硝基三氟甲苯的循环两阶段硝化方法

    公开(公告)号：US4096195A

    公开(公告)日：1978-06-20

    申请号：US796519

    申请日：1977-05-13

    Applicant: Louis Schneider ,  David E. Graham

    Inventor： Louis Schneider ,  David E. Graham

    IPC: C07C67/00 ,  C07C201/00 ,  C07C205/12 ,  C07C79/12

    CPC classification number: C07C201/08 ,  C07C201/14

    Abstract: In accordance with the present invention, there is provided herein a cyclic, two-stage process for dinitrating 4-chlorobenzotrifluoride to form 4-chloro-3,5-dinitrobenzotrifluoride in high yield. The process commences with a mononitration stage wherein 4-chlorobenzotrifluoride is substantially completely converted to 4-chloro-3-nitrobenzotrifluoride (the "monoitro" compound) in the presence of a nitric acid, sulfur trioxide and sulfuric acid mixture. The used acid mixture then is diluted with water to form an aqueous used acid layer in which the solubility of the mononitro compound is negligible and a mononitro layer. The aqueous used acid layer then is separated from the mononitro layer and discarded. The mononitro compound thereafter is further nitrated in a dinitration stage in the presence of a fresh nitric acid, sulfur trioxide and sulfuric acid mixture. The fresh acid mixture contains an excess of nitric acid sufficient to carry out both nitrations using the partially spent acid mixture of the dinitration stage as the acid mixture for the mononitration stage. The reaction product of the dinitration stage is the desired dinitro compound and a partially spent acid mixture, which contains some dinitro compound dissolved therein. The dinitro layer then is separated from the partially spent acid layer and recovered and the acid layer is recycled back to the mononitration stage.

    Abstract translation: 根据本发明，本文提供了一种用于将4-氯三氟甲苯二硝基化以环状二步法，以高产率形成4-氯-3,5-二硝基三氟甲苯。 该过程开始于硝酸，三氧化硫和硫酸混合物存在下，4-氯三氟甲苯基本上完全转化为4-氯-3-硝基三氟甲苯（“一硝基”化合物）的单硝化阶段。 然后将所使用的酸混合物用水稀释以形成其中单硝基化合物的溶解度可忽略的水性使用的酸层，和单硝酸层。 然后将水性使用的酸层与单硝基层分离并丢弃。 此后的单硝基化合物在新硝酸，三氧化硫和硫酸混合物的存在下，在二硝化阶段进一步硝化。 新鲜的酸性混合物含有足够多的硝酸，使用二硝化阶段的部分废酸混合物作为单硝化阶段的酸混合物进行硝化。 二硝化阶段的反应产物是所需的二硝基化合物和部分废酸混合物，其中含有一些溶解在其中的二硝基化合物。 然后将二硝基层与部分废酸层分离并回收，酸层再循环回到单硝化阶段。

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