Process for the preparation of insecticidal phenylhydrazine derivatives
    56.
    发明授权
    Process for the preparation of insecticidal phenylhydrazine derivatives 有权
    杀虫剂苯肼衍生物的制备方法

    公开(公告)号:US06278022B1

    公开(公告)日:2001-08-21

    申请号:US09431197

    申请日:1999-11-01

    Applicant: Haihong Jin

    Inventor: Haihong Jin

    Abstract: Disclosed herein is an improvement in a method for making compounds having the structural formulae (I) or (II): wherein: X is a) phenyl; lower phenylalkoxy; phenoxy; or benzyl; or b) one substituent from group a) and one or more substituents selected from C1-C4 alkoxy; hydroxyl; halogen; lower alkyl; and lower alkylthio; or c) along with the phenyl to which it is attached, forms a multiple fused ring heterocycle such as dibenzofuranyl; Y is H, C1-C4 alkanoyl, C1-C4 haloalkenoyl, dialkoxyphosphoryl, alkylaminocarbonyl, haloalkylsulfonyl, or C1-C4 alkoxy carbonyl; and R is H, C1-C6 alkyl, C1-C6 alkoxy, C3-C6 cycloalkoxy, haloalkyl, alkoxyalkyl, arylalkoxy, alkenyl, alkylthio, alkoxycarbonyl, alkylamino, heteroaryl, arylalkyl, haloalkoxy, aryloxy, or C3-C6 cycloalkyl; and Z is O or S, wherein the improvement comprises the steps of: A) selecting as a starting material a compound of the structural formula B) dissolving compound III in an organic solvent selected from the group consisting of methyl t-butyl ether, ethylene glycol dimethyl ether, 2-methoxyethyl ether, acetonitrile, and acetic acid, and C) nitrating with nitric acid to form a compound of the structural formula

    Abstract translation: 本文公开了具有结构式(I)或(II)的化合物的制备方法的改进:其中:X为a)苯基; 低级苯基烷氧基; 苯氧基 或苄基; 或b)a)中的一个取代基和一个或多个选自C 1 -C 4烷氧基的取代基; 羟; 卤素; 低级烷基 和低级烷硫基; 或c)与其连接的苯基一起形成多重稠环杂环,例如二苯并呋喃基; Y是H,C 1 -C 4烷酰基,C 1 -C 4卤代烯酰基,二烷氧基磷酰基,烷基氨基羰基,卤代烷基磺酰基或C 1 -C 4烷氧基羰基; C 1 -C 6烷基,C 1 -C 6烷氧基,C 3 -C 6环烷氧基,卤代烷基,烷氧基烷基,芳基烷氧基,烯基,烷硫基,烷氧基羰基,烷基氨基,杂芳基,芳烷基,卤代烷氧基,芳氧基或C 3 -C 6环烷基; 并且Z为O或S,其中改进包括以下步骤:A)将化合物III溶于选自甲基叔丁基醚,乙二醇的有机溶剂中的结构式B)化合物作为起始原料 二甲醚,2-甲氧基乙醚,乙腈和乙酸,和C)用硝酸硝化形成结构式的化合物

    Method for treating aqueous solutions comprising acids and nitrated compounds
    57.
    发明授权
    Method for treating aqueous solutions comprising acids and nitrated compounds 有权
    用于处理包含酸和硝化化合物的水溶液的方法

    公开(公告)号:US06254789B1

    公开(公告)日:2001-07-03

    申请号:US09485498

    申请日:2000-05-03

    Abstract: The invention concerns a method for treating an aqueous solution derived from sluicing of crude mononitrated or dinitrated aromatic compounds obtained by nitration of the corresponding aromatic compounds, consisting in: (a) contacting said aqueous solution with said aromatic compound thereby obtaining an aqueous phase and an organic phase; (b) recycling said organic phase in the nitration process; (c) distilling said aqueous phase; (d) recycling the resulting concentrated acid solution in the nitration process; (e) recycling or eliminating the recuperated water after distillation.

    Abstract translation: 本发明涉及一种处理衍生自通过硝化相应芳族化合物而得到的粗单硝化或二硝化芳族化合物的水溶液的方法,其包括:(a)使所述水溶液与所述芳族化合物接触,从而获得水相和 有机相; (b)在硝化过程中回收所述有机相; (c)蒸馏所述水相; (d)在硝化过程中回收所得浓酸溶液; (e)蒸馏后回收或除去回收的水。

    Recovering/recycling nitric acid from dinitration process streams comprising HNO3/dinitro compounds
    58.
    发明授权
    Recovering/recycling nitric acid from dinitration process streams comprising HNO3/dinitro compounds 失效
    从包含HNO3 /二硝基化合物的二硝化工艺流中回收/再循环硝酸

    公开(公告)号:US06191325B1

    公开(公告)日:2001-02-20

    申请号:US09130348

    申请日:1998-08-13

    CPC classification number: C07C201/16 C07C201/08 C07C205/06

    Abstract: Dinitro aromatic compounds are improvedly prepared by reacting an aromatic compound with a nitric acid nitrating agent and thence separating the nitrating acid from the process stream thus formed, the process stream containing said at least one dinitro aromatic compound and also having a fraction of the nitrating acid dissolved therein, the subject process also comprising (a) distilling/stripping nitric acid from said process stream, (b) recovering nitric acid from the top of the distillation/stripping vessel and recycling same to the nitration reaction and (c) washing the process stream which contains the at least one dinitro aromatic compound, but having the nitric acid removed therefrom.

    Abstract translation: 二硝基芳族化合物通过使芳族化合物与硝酸硝化剂反应,然后从所形成的工艺流中分离硝酸而改进制备,所述工艺流含有所述至少一种二硝基芳族化合物,并且还含有一部分硝酸 本方法还包括(a)从所述工艺流中蒸馏/除去硝酸,(b)从蒸馏/汽提容器的顶部回收硝酸并将其再循环到硝化反应,和(c)洗涤该过程 其含有至少一种二硝基芳族化合物,但其中除去硝酸。

    Preparation of picric acid
    60.
    发明授权
    Preparation of picric acid 失效
    苦味酸的制备

    公开(公告)号:US6063967A

    公开(公告)日:2000-05-16

    申请号:US94595

    申请日:1998-06-15

    CPC classification number: C07C201/16 C07C201/08

    Abstract: Picric acid, namely, 2,4,6-trinitrophenol, is readily and effectively prepared by nitrating o-nitrophenol and/or p-nitrophenol into at least one dinitrophenol in a nitric acid medium of reaction, characteristically essentially consisting of nitric acid or immixture thereof with a strong co-acid, the at least one dinitrophenol remaining soluble in the medium of reaction, and therein completing nitration of the at least one dinitrophenol and precipitating picric acid therefrom.

    Abstract translation: 苦味酸,即2,4,6-三硝基苯酚,通过在硝酸反应介质中将邻硝基苯酚和/或对硝基苯酚硝化成至少一种二硝基酚而容易且有效地制备,其特征在于主要由硝酸或杂质组成 其中所述至少一种二硝基苯酚仍然可溶于所述反应介质中,并且其中完成所述至少一种二硝基苯酚的硝化并从其沉淀出苦味酸。

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