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    • 72. 发明公开
    • Large scale batch process for diazomethane
    • 批量大法维尔法赫尔斯特隆von Diazomethan
    • EP0916649A1
    • 1999-05-19
    • EP98203801.0
    • 1998-11-11
    • AEROJET-GENERAL CORPORATION
    • Archibald, Thomas G.Huang, Der-ShingPratton, Mark H.Barnard, James C.
    • C07C245/16
    • C07C245/16
    • Diazomethane is prepared in a batch process on a scale of at least 50 gram-moles per batch, from an N-methyl-N-nitroso amine in an organic solvent and an inorganic base in an aqueous solution by the use of a phase transfer catalyst and by controlling the choice of solvent, reagent concentrations, addition rate and reaction temperature to cause codistillation of the product and the organic solvent in such a manner that the concentration of diazomethane in both liquid and vapor phases are controlled within limits that will prevent detonation of the diazomethane.
    • 重氮甲烷的制备包括:(a)在有机溶剂中加入至少约50g摩尔的式(I)的N-甲基-N-亚硝基胺的溶液,其中:(i)当与 水; 和(ii)相对于含有相对于(I)的过量无机碱的水溶液的反应容器和相转移催化剂,沸点低于约40℃,同时将反应容器的内容物保持在 足以使由此形成的有机溶剂和重氮甲烷蒸发的温度,(I)的加入速率和反应容器的温度保持使得反应容器中的液相中的重氮甲烷浓度保持在3重量% 所生成的气相中的重氮甲烷浓度保持在约25摩尔%以下; 和(b)冷凝形成的气相,得到重氮甲烷的有机液体溶液。 R =吸电子基团。