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    Purification process
    321.
    发明授权
    Purification process 失效
    净化过程

    公开(公告)号：US6072080A

    公开(公告)日：2000-06-06

    申请号：US41858

    申请日：1998-03-12

    Applicant: Louie Akos Nady ,  Seyed Mehdi Tavana ,  Thomas Gray ,  Stephen Martin Brown ,  Brian David Gott

    Inventor： Louie Akos Nady ,  Seyed Mehdi Tavana ,  Thomas Gray ,  Stephen Martin Brown ,  Brian David Gott

    IPC: C07C201/16 ,  C07C205/00

    CPC classification number: C07C201/16 ,  C07C311/51

    Abstract: A process for the purification of a compound of general formula I: ##STR1## wherein R.sup.1 is hydrogen or C.sub.1 -C.sub.6 alkyl, C.sub.2 -C.sub.6 alkenyl or C.sub.2 -C.sub.6 alkynyl, any of which may optionally be substituted with one or more substituents selected from halogen and hydroxy; or COOR.sup.4, COR.sup.6, CONR.sup.4 R.sup.5 or CONHSO.sub.2 R.sup.4 ;R.sup.4 and R.sup.5 independently represent hydrogen or C.sub.1 -C.sub.4 alkyl optionally substituted with one or more halogen atoms;R.sup.6 is a halogen atom or a group R.sup.4 ;R.sup.2 is hydrogen or halo; andR.sup.3 is C.sub.1 -C.sub.4 alkyl, C.sub.2 -C.sub.4 alkenyl or C.sub.2 -C.sub.4 alkynyl, any of which may optionally be substituted with one or more halogen atoms; or halo;or, where appropriate, a salt thereof;from a mixture containing the compound of general formula I together with one or more isomers or di-nitrated analogues thereof; the process comprising dissolving the mixture in a suitable crystallisation solvent and recrystallising the product from the resulting crystallisation solution wherein the crystallisation solution contains not more than 25% loading of the compound of general formula I, loading being defined as: ##EQU1## and wherein the temperature to which the solution is cooled for crystallisation is not greater than about 30.degree. C.; wherein, after the addition of the crystallising solvent but before recrystallisation, the crystallisation solution is subjected to at least one wash with an aqueous solution having an acid pH followed by back extraction with fresh crystallising solvent. The process is particularly useful for purifying acifluorfen produced via a route starting with m-cresol.

    Abstract translation: 一种用于纯化通式I化合物的方法：其中R 1是氢或C 1 -C 6烷基，C 2 -C 6烯基或C 2 -C 6炔基，其中任何一个可任选被一个或多个选自卤素和羟基的取代基取代 ; 或COOR4，COR6，CONR4R5或CONHSO2R4; R4和R5独立地表示氢或任选被一个或多个卤素原子取代的C 1 -C 4烷基; R6是卤素原子或基团R4; R2是氢或卤素; 并且R 3是C 1 -C 4烷基，C 2 -C 4烯基或C 2 -C 4炔基，其中任何一个可任选地被一个或多个卤素原子取代; 或卤素; 或者在适当情况下为其盐; 从含有通式I化合物的混合物与一种或多种异构体或其二硝化类似物组合; 该方法包括将该混合物溶解在合适的结晶溶剂中，并从所得结晶溶液中重结晶该产物，其中该结晶溶液含有不超过25％的通式I化合物的负载量，其定义为：并且其中 该溶液冷却结晶不大于约30℃; 其中，在加入结晶溶剂之后但在重结晶之前，将结晶溶液用具有酸性pH的水溶液进行至少一次洗涤，然后用新鲜的结晶溶剂反萃取。 该方法特别可用于纯化通过以间甲酚开始的途径产生的三氟果霜。

    Method of separating isomers of nitrotoluic acid
    322.
    发明授权
    Method of separating isomers of nitrotoluic acid 失效
    分离硝基甲酸异构体的方法

    公开(公告)号：US6054609A

    公开(公告)日：2000-04-25

    申请号：US194018

    申请日：1998-11-19

    Applicant: Keiichi Yokota ,  Ikuo Ito ,  Seiji Takeuchi

    Inventor： Keiichi Yokota ,  Ikuo Ito ,  Seiji Takeuchi

    IPC: C07C201/16 ,  C07C205/57 ,  C07C205/06

    CPC classification number: C07C201/16

    Abstract: A method of separating 3-nitro-o-toluic acid and 5-nitro-o-toluic acid from a mixture of said isomers, comprising producing salts by adding an aromatic organic base, for example, aniline or pyridine, to the said mixture, separating said salts into solids and a mother liquor, by taking advantage of the difference in solubilities between the said salts to water or a mixed solvent consisting of water and a water-soluble organic compound, for example, methanol, and, further, recovering 3-nitro-o-toluic acid from the mother liquor and 5-nitro-o-toluic acid from the solids.

    Abstract translation: PCT No.PCT / JP98 / 00277 Sec。 371日期：1998年11月19日 102（e）1998年11月19日日期PCT 1998年1月26日PCT PCT。 出版物WO98 / 42654 日期1998年10月1日从所述异构体的混合物中分离出3-硝基邻甲苯甲酸和5-硝基邻甲苯甲酸的方法，包括通过加入芳族有机碱例如苯胺或吡啶来制备盐， 通过利用所述盐与水或由水和水溶性有机化合物（例如甲醇）组成的混合溶剂之间的溶解度的差异，将所述盐分离成固体和母液，并且 进一步从母液中回收3-硝基 - 邻甲苯甲酸，从固体中回收5-硝基 - 邻甲苯甲酸。

    Process for the preparation of 5-fluoro-2-nitrobenzoic acid
    323.
    发明授权
    Process for the preparation of 5-fluoro-2-nitrobenzoic acid 失效
    5-氟-2-硝基苯甲酸的制备方法

    公开(公告)号：US5756831A

    公开(公告)日：1998-05-26

    申请号：US667833

    申请日：1996-06-20

    Applicant: Wolfram Kissener ,  Jurgen Kuprat ,  Herbert Emde ,  Klaus-Christian Paetz

    Inventor： Wolfram Kissener ,  Jurgen Kuprat ,  Herbert Emde ,  Klaus-Christian Paetz

    IPC: C07C201/08 ,  C07C201/16 ,  C07C205/58

    CPC classification number: C07C201/08

    Abstract: 5-Fluoro-2-nitrobenzoic acid having low contents of 3-fluoro-2-nitro-benzoic acid is prepared in a simple manner by nitrating 3-fluorobenzoic acid in an anhydrous medium using an anhydrous nitrating acid and isolating and purifying 5-fluoro-2nitro-benzoic acid, by taking 7.5 to 15 parts by weight of water, based on 1 part by weight of 3-fluorobenzoic acid used, introducing the reaction mixture reacted to exhaustion into this volume of water taken, filtering off the precipitate formed and washing it with water.

    Abstract translation: 通过使用无水硝酸将氮氟酸在无水介质中硝化3-氟苯甲酸，分离纯化5-氟-2-硝基苯甲酸，得到3-氟-2-硝基 - 苯甲酸含量低的5-氟-2-硝基苯甲酸 -2-硝基 - 苯甲酸，通过使用7.5重量份水，以1重量份所用的3-氟苯甲酸为原料，将反应混合物反应至该体积的水中，滤出形成的沉淀物， 用水冲洗。

    Process for the production of dinitrobenzene and mononitrobenzene
    325.
    发明授权
    Process for the production of dinitrobenzene and mononitrobenzene 失效
    生产二硝基苯和单硝基苯的方法

    公开(公告)号：US5488187A

    公开(公告)日：1996-01-30

    申请号：US290575

    申请日：1994-08-15

    Applicant: Robert W. Mason

    Inventor： Robert W. Mason

    IPC: C07C201/08 ,  C07C201/16 ,  C07C205/06

    CPC classification number: C07C201/08 ,  C07C201/16

    Abstract: Aromatic nitration reactions and, more specifically, a process for nitrating benzene to produce dinitrobenzene or mononitrobenzene in the absence of sulfuric acid and in the absence of any dipolar aprotic solvent.

    Abstract translation: 更具体地说，是在不存在硫酸的情况下和在不存在任何偶极非质子溶剂的情况下硝化苯以产生二硝基苯或单硝基苯的方法。

    Method of preparing 4-trifluoromethyl-2-nitrobenzoic acid and novel isomer
    330.
    发明授权
    Method of preparing 4-trifluoromethyl-2-nitrobenzoic acid and novel isomer 失效
    制备4-三氟甲基-2-硝基苯甲酸和新异构体的方法

    公开(公告)号：US4845279A

    公开(公告)日：1989-07-04

    申请号：US136715

    申请日：1987-12-22

    Applicant: Yasunori Nishimura ,  Yoshihiko Gotoh ,  Toshikazu Kawai

    Inventor： Yasunori Nishimura ,  Yoshihiko Gotoh ,  Toshikazu Kawai

    IPC: C07B63/02 ,  C07C67/00 ,  C07C201/00 ,  C07C201/08 ,  C07C201/16 ,  C07C205/58

    CPC classification number: C07C201/16 ,  C07C205/58

    Abstract: An isomer mixture of 4-trifluoromethyl-2-nitrobenzoic acid and 4-trifluoromethyl-3-nitrobenzoic acid, which is a novel compound, is obtained by nitrating a compound represented by ##STR1## (Z is COY or CY.sub.3, and Y is a halogen atom) with a nitrating agent comprising nitric acid and simultaneously hydrolyzing the radical Z. Each of the two isomers is easily isolated by treating the mixture with a basic neutralizing agent to obtain a solution containing the 2-nitro isomer and a precipitate containing the 3-nitro isomer.

    Abstract translation: 通过将由下式表示的化合物（Z是COY或CY3，Y是一个或多个）来获得，作为新化合物的4-三氟甲基-2-硝基苯甲酸和4-三氟甲基-3-硝基苯甲酸的异构体混合物 卤素原子）与含硝酸的硝化剂同时水解基团Z.通过用碱性中和剂处理混合物容易地分离出两种异构体，得到含有2-硝基异构体的溶液和含有3 - 硝基异构体。

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