Process for the preparation of 2-nitrobenzaldehyde
    82.
    发明授权
    Process for the preparation of 2-nitrobenzaldehyde 失效
    制备2-硝基苯甲醛的方法

    公开(公告)号:US4297519A

    公开(公告)日:1981-10-27

    申请号:US125617

    申请日:1980-02-28

    申请人: Werner Ertel

    发明人: Werner Ertel

    CPC分类号: C07C201/12 C07C201/16

    摘要: A process provided for the production of 2-nitrobenzaldehyde from 2-nitrotoluene, in which 2-nitrotoluene is converted, by bromination by a radical mechanism, to 2-nitrobenzyl bromide in the form of a bromination oil containing 20 to 50% or more of 2-nitrobenzyl bromide, and the bromination oil is oxidized directly with a mixture of dimethylsulphoxide and sodium bicarbonate in a weight ratio of 3:1 to 10:1 at temperatures of up to 100.degree. C. and the 2-nitrobenzaldehyde is subsequently isolated via the bisulphite adduct, to give 2-nitrobenzaldehyde in high purity and high yield. The process also has the advantage of a very short reaction time. The 2-nitrobenzaldehyde produced is an important intermediate, for example in the production of pharmaceutically active 1,4-dihydropyridines.

    摘要翻译: 通过自由基机理的溴化将2-硝基甲苯转化为2-硝基甲苯的2-硝基苯甲醛制备为含有20〜50%以上的溴化油形式的2-硝基苄基溴的方法, 2-硝基苄基溴,溴化油直接用二甲基亚砜和碳酸氢钠的混合物以3:1至10:1的重量比在高达100℃的温度下氧化,然后将2-硝基苯甲醛通过 亚硫酸氢盐加合物,得到2-硝基苯甲醛,纯度高,产率高。 该方法还具有非常短的反应时间的优点。 产生的2-硝基苯甲醛是重要的中间体,例如在制备药物活性的1,4-二氢吡啶中。

    Preparation of aromatic fluoro compounds
    84.
    发明授权
    Preparation of aromatic fluoro compounds 失效
    芳香族氟化合物的制备

    公开(公告)号:UST993005I4

    公开(公告)日:1980-04-01

    申请号:US22597

    申请日:1979-03-19

    摘要: The present invention relates to a process for the preparation of 4,4'-difluorobenzophenone. 4,4-difluorobenzophenone may be prepared by diazotization of 4,4'-diamino-diphenylmethane in anhydrous or concentrated aqueous hydrogen fluoride, decomposition of the diazonium fluoride thus produced to yield 4,4'-difluoro-diphenylmethane and oxidation of 4,4'-difluoro-diphenylmethane to yield 4,4'-difluorobenzophonone.Thus, according to the present invention, there is provided a process for the preparation of 4,4'-difluorobenzophenone which comprises the following steps:(1) diazotization of 4,4'-diamino-diphenylmethane in anhydrous or concentrated aqueous hydrogen fluoride to yield a solution of a corresponding diazonium fluoride; and(2) (i) thermally decomposing the diazonium fluoride in the solution thus produced to yield 4,4'-difluoro-diphenylmethane and (ii) subsequently oxidizing the 4,4'-difluoro-diphenylmethane to yield 4,4'-difluorobenzophenone.

    Arylperfluoroalkanes
    89.
    发明授权
    Arylperfluoroalkanes 失效
    芳基全氟烷烃

    公开(公告)号:US4071570A

    公开(公告)日:1978-01-31

    申请号:US659624

    申请日:1976-02-20

    摘要: New fluoro derivatives of aralkylamine compounds, particularly 2-(2-phenyl-1,1,2,2-tetrafluoroethyl)benzylamine, as well as the N-alkyl and the N,N-dialkyl derivatives thereof are prepared by reaction of 2-bromobenzonitrile with benzylmagnesium chloride to produce 2'-bromo-2-phenylacetophenone; oxidation of said acetophenone with selenous acid to produce 2-bromobenzil; conversion of the benzil compound by treatment with sulfur tetrafluoride to the corresponding 2-bromo-.alpha.,.alpha.-.alpha.',.alpha.'-tetrafluorobibenzyl;followed by reaction of the 2-bromobibenzyl compound with a metal cyanide to produce the corresponding 2-(2-phenyl-1,1,2,2-tetrafluoroethyl)benzonitrile. This nitrile compound is then reduced with lithium aluminum hydride to produce the corresponding benzylamine, which is then converted, if desired, to the N-alkyl and/or N,N-dialkyl 2-(2-phenyl-1,1,2,2-tetrafluoroethyl)benzylamine. Alternatively, the nitrile or the precursor bromobibenzyl can be converted by Grignard reactions to the corresponding .alpha.-alkyl or .alpha.,.alpha.-dialkylbenzylamine which can then be converted if desired to the corresponding N-alkyl and/or N,N-dialkyl substituted benzylamine compound. The phenyltetrafluoroethylbenzylamine as well as its N-alkyl and N,N-dialkyl derivatives are active as antiarrhythmic agents.

    摘要翻译: 芳烷基胺化合物,特别是2-(2-苯基-1,1,2,2-四氟乙基)苄胺以及N-烷基和N,N-二烷基衍生物的新的氟衍生物通过2- 溴苄腈与苄基氯化镁反应生成2'-溴-2-苯基苯乙酮; 用硒酸氧化所述苯乙酮以产生2-溴苯甲醇; 通过用四氟化硫处理将苯偶酰化合物转化成相应的2-溴-α,α-α',α'-四氟联苄;然后将2-溴苄基化合物与金属氰化物反应,生成相应的2-(2 苯基-1,1,2,2-四氟乙基)苄腈。 然后将该腈化合物用氢化铝锂还原以产生相应的苄胺,然后如果需要将其转化为N-烷基和/或N,N-二烷基2-(2-苯基-1,1,2, 2-四氟乙基)苄胺。 或者,腈或前体溴联苄可以通过格利雅反应转化成相应的α-烷基或α,α-二烷基苄基胺,如果需要,可以将其转化成相应的N-烷基和/或N,N-二烷基取代的苄胺化合物 。 苯基四氟乙基苄胺以及其N-烷基和N,N-二烷基衍生物作为抗心律不齐剂是有活性的。