Process for the preparation of fluorinated nitroalkanes
    42.
    发明授权
    Process for the preparation of fluorinated nitroalkanes 失效
    制备氟化硝基烷烃的方法

    公开(公告)号:US4518812A

    公开(公告)日:1985-05-21

    申请号:US575636

    申请日:1984-01-31

    CPC classification number: C07C201/14 C07C205/08

    Abstract: In the conjugated nitrofluorination of an olefin by reacting an olefin of the formula ##STR1## in which R.sup.1, R.sup.2, R.sup.3 and R.sup.4 each independently is hydrogen, fluorine, chlorine, bromine, alkyl, halogenoalkyl or cycloalkyl, orR.sup.2 and R.sup.4 together are an alkylene radical of 3 to 6 carbon atoms,with hydrogen fluoride and nitric acid to produce an .alpha.-fluorinated nitroalkane of the formula ##STR2## the improvement which comprises effecting the reaction in a vessel protected against corrosion employing about 1 to 1.1 mols of hydrogen fluoride and about 1 to 2 mols of nitric acid per mol of olefin. The process uses much less HF than heretofore and the products are useful intermediates in making herbicides. Some of the products are new.

    Abstract translation: 在烯烃的共轭硝基氟化中,通过使式(IMAGE)的烯烃反应,其中R 1,R 2,R 3和R 4各自独立地是氢,氟,氯,溴,烷基,卤代烷基或环烷基,或者R 2和R 4一起是 具有3至6个碳原子的亚烷基,与氟化氢和硝酸反应以产生下式的α-氟化的硝基烷烃:其中包括在使用约1至1.1摩尔氟化氢的保护反应的容器中进行反应 和约1至2摩尔硝酸/摩尔烯烃。 该方法使用比迄今为止少得多的HF,并且该产品是制备除草剂的有用中间体。 一些产品是新的。

    Process for preparing 1-nitrobenzene-2-alkyloxycarbonyl-5-carboxylic
acids
    43.
    发明授权
    Process for preparing 1-nitrobenzene-2-alkyloxycarbonyl-5-carboxylic acids 失效
    制备1-硝基苯-2-烷氧基羰基-5-羧酸的方法

    公开(公告)号:US4507491A

    公开(公告)日:1985-03-26

    申请号:US445008

    申请日:1982-11-29

    CPC classification number: C07C201/14

    Abstract: To prepare a 1-nitrobenzene-2-alkyloxycarbonyl-5-carboxylic acid, a dialkyl benzene-1,4-dicarboxylate is first nitrated in a customary manner and the dialkyl 1-nitrobenzene-2,5-dicarboxylate compound obtained is subjected to a partial acidic ester hydrolysis without isolating the nitro compound prepared as an intermediate. The acidic ester hydrolysis is carried out in the presence of a catalytic amount of an organic solvent which is completely or partially miscible with water and has a boiling point of above 90.degree. C. and/or of an emulsifier; it is preferably carried out at a temperature between 65.degree. and 110.degree. C.

    Abstract translation: 为了制备1-硝基苯-2-烷氧基羰基-5-羧酸,以常规方式首先硝化二苯基-1,4-二羧酸二烷基酯,将得到的1-硝基苯-2,5-二羧酸二烷基酯化合物 不分离作为中间体制备的硝基化合物的部分酸性酯水解。 酸性酯水解在催化量的与水完全或部分混溶并且沸点高于90℃的有机溶剂和/或乳化剂的存在下进行; 优选在65℃〜110℃的温度下进行。

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