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    Process for the preparation of fluorinated nitroalkanes
    94.
    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

    申请人： Bernd Baasner ,  Hermann Hagemann ,  Erich Klauke

    发明人： Bernd Baasner ,  Hermann Hagemann ,  Erich Klauke

    IPC分类号： C07C67/00 ,  C07C201/00 ,  C07C201/14 ,  C07C205/08 ,  C07C76/02 ,  C07C79/02

    CPC分类号： C07C201/14 ,  C07C205/08

    摘要： 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.

    摘要翻译： 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 producing N-chlorocarbonyl isocyanide dichloride
    100.
    发明授权
    Process for producing N-chlorocarbonyl isocyanide dichloride 失效
    制备N-氯羰基异腈二氯化物的方法

    公开(公告)号：US3956089A

    公开(公告)日：1976-05-11

    申请号：US544021

    申请日：1975-01-24

    申请人： Hermann Hagemann ,  Herbert Schwarz ,  Fritz Doring

    发明人： Hermann Hagemann ,  Herbert Schwarz ,  Fritz Doring

    IPC分类号： C07C271/00 ,  C07C20060101 ,  C07C67/00 ,  C07C239/00 ,  B01J1/10

    摘要： N-chlorocarbonyl isocyanide dichloride is prepared by chlorinating methyl isocyanate and/or methyl carbamic acid chloride in solution in the presence of ultraviolet light at a temperature in the range of from 30.degree. to 120.degree.C. The temperature pattern during the reaction is controlled in relation to the concentration of methyl isocyanate in the reaction mixture such that low temperatures are maintained for high concentrations while high temperatures are maintained with low concentrations. Thus, when a temperature of from 30.degree.-40.degree.C is maintained during the reaction, the concentration of methyl isocyanate in the reaction mixture is substantially more than 50 percent; when the temperature is increased to 65.degree. to 75.degree.C, the concentration of methyl isocyanate is in the range of 50 percent to 10 percent; and when the temperature is increased above 75.degree.C, the concentration of methyl isocyanate is substantially below 10 percent.

    摘要翻译： 氯化异氰酸甲酯和/或甲基氨基甲酸氯化物在紫外线的存在下，在30〜120℃的温度范围内，通过氯化甲基氨基甲酰氯来制备N-氯羰基异氰化物二氯化物。反应过程中的温度控制在 与反应混合物中甲基异氰酸酯的浓度的关系，使得在高浓度下保持低温保持高浓度，同时以低浓度保持高温。 因此，当反应期间保持30〜40℃的温度时，反应混合物中甲基异氰酸酯的浓度大致超过50％; 当温度升高至65℃至75℃时，异氰酸甲酯的浓度在50％至10％的范围内; 当温度升高到75℃以上时，异氰酸甲酯的浓度显着低于10％。