Process for the preparation of 2-[alkyl(aryl)]sulfonylbenzene-sulfonyl chlorides and their intermediates
    20.
    发明授权
    Process for the preparation of 2-[alkyl(aryl)]sulfonylbenzene-sulfonyl chlorides and their intermediates 失效
    2- [烷基(芳基)]磺酰基苯磺酰氯及其中间体的制备方法

    公开(公告)号:US06642416B2

    公开(公告)日:2003-11-04

    申请号:US10285067

    申请日:2002-10-31

    IPC分类号: C07C30978

    摘要: A process for the preparation of 2-[alkyl(aryl)]sulfonylbenzene sulfonyl chlorides of the following formula is provided: in which R is alkyl or aryl substituted at the ortho or meta positions with alkyl, aryl, NHAc or alkoxy, comprising the steps of: a) reacting 2-chloronitrobenzene, 2-fluoronitrobenzene or 2-bromonitrobenzene with a compound of the following formula: RSO2−M+ wherein R is defined above; and M is sodium, potassium, lithium, ammonium or quaternary ammonium, in a polar aprotic solvent at a temperature of about 50 to 190° C.; b) reacting the material prepared in step (a) with hydrogen at a pressure of about 20 to about 60 psi in a polar aprotic solvent at a temperature of about 20 to about 60° C.; and c) diazotizing the material prepared in step (b) with sodium nitrite in the presence of hydrochloric acid and reacting the resulting diazonium salt with sulfur dioxide in the presence of copper (I) or copper (II) compounds or a mixture thereof, in water.

    摘要翻译: 提供了制备下式的2- [烷基(芳基)]磺酰基苯磺酰氯的方法:其中R是在邻位或间位被烷基,芳基,NHAc或烷氧基取代的烷基或芳基,其包括步骤 :a)使2-氯硝基苯,2-氟硝基苯或2-溴硝基苯与下式化合物反应:其中R定义如上; 在极性非质子溶剂中,在约50至190℃的温度下,将M是钠,钾,锂,铵或季铵; b)使步骤(a)中制备的材料与约20℃压力的氢反应 在约20至约60℃的温度下在极性非质子溶剂中至约60psi。 和c)在盐酸存在下用亚硝酸钠在步骤(b)中制备的材料重氮化,并在铜(I)或铜(II)化合物或其混合物的存在下,在水中使所得重氮盐与二氧化硫反应 。