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    • 3. 发明授权
    • Process for preparing N,O-disubstituted hydroxylamine compounds
    • 制备N,O-二取代羟胺化合物的方法
    • US5371264A
    • 1994-12-06
    • US9528
    • 1993-01-27
    • James A. MannerSuresh B. Damle
    • James A. MannerSuresh B. Damle
    • C07C239/22C07C269/04C07C271/00C07C275/64C07C69/96
    • C07C275/64C07C239/22C07C269/04C07C271/00
    • Describes a process for preparing N,O-disubstituted hydroxylamine compounds comprising reacting an aqueous solution of free hydroxylamine with an equimolar amount of a carbonyl halide-containing compound, e.g., a chloroformate such as phenyl chloroformate, in the presence of a substantially stoichiometric amount of a weak inorganic basic reagent, thereby to produce the N-substituted derivative, and thereafter further reacting an inert organic solvent solution of the N-substituted derivative with an equimolar amount of the corresponding carbonyl halide-containing compound in the presence of a substantially stoichiometric amount of weak inorganic basic reagent, thereby to produce the N,O-disubstituted derivative, e.g., N,O-bis(phenoxycarbonyl) hydroxylamine. In a preferred embodiment, the organic solvent is used also in the reaction that produces the N-substituted derivative. N,O-disubstituted hydroxylamine compounds containing less than 3 weight percent, e.g., less than 0.5 weight percent, of the hydrolysis by-product of the carbonyl halide-containing compound may be produced thereby.
    • 描述了制备N,O-二取代的羟胺化合物的方法,包括使游离羟胺的水溶液与等摩尔量的含羰基卤化合物,例如氯甲酸酯如氯甲酸苯酯,在基本上化学计量的 弱的无机碱性试剂,从而产生N-取代的衍生物,然后在基本上化学计量的存在下,使N-取代的衍生物的惰性有机溶剂溶液与等摩尔量的相应的含羰基卤化合物进一步反应 的弱无机碱性试剂,从而产生N,O-二取代的衍生物,例如N,O-双(苯氧基羰基)羟胺。 在优选的实施方案中,有机溶剂也用于产生N-取代的衍生物的反应中。 因此可以制备含有小于3重量%,例如小于0.5重量%的含羰基卤化合物的水解副产物的N,O-二取代羟胺化合物。