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    Process for preparing N,O-dialkylhydroxylamine, its salts or intermediates in their synthesis
    5.
    发明授权
    Process for preparing N,O-dialkylhydroxylamine, its salts or intermediates in their synthesis 失效
    在其合成中制备N，O-二烷基羟胺，其盐或中间体的方法

    公开(公告)号：US5510511A

    公开(公告)日：1996-04-23

    申请号：US97225

    申请日：1993-07-27

    申请人： Satoshi Inoki ,  Mitsuyuki Takesue ,  Isao Hashimoto ,  Noriaki Kihara ,  Kiyoaki Sugi

    发明人： Satoshi Inoki ,  Mitsuyuki Takesue ,  Isao Hashimoto ,  Noriaki Kihara ,  Kiyoaki Sugi

    IPC分类号： C07C239/20 ,  C07C271/12 ,  C07C261/00

    CPC分类号： C07C271/12 ,  C07C239/20

    摘要： A process for preparing N,O-dialkylhydroxycarbamic acid ester which comprises reacting hydroxylamine or its salt with dihydrocarbyl carbonate in the presence of a basic compound to prepare hydroxycarbamic acid ester and subsequently alkylating this compound with an alkylating agent; a process for recovering N,O-dialkylhydroxycarbamic acid ester which comprises azeotropically distilling the ester with water from a solution containing the ester; a process for preparing N,O-dialkylhydroxylamine which comprises hydrolyzing N,O-dialkylhydroxycarbamic acid ester in an aqueous solution or a hydrous solvent in the presence of an alkali; a process for purifying N,O-dialkylhydroxylamine hydrochloride which comprises adding aldehyde or ketone to a solution of N,O-dialkylhydroxylamine hydrochloride containing O-alkylhydroxylamine hydrochloride as impurities to convert the O-alkylhydroxylamine hydrochloride into O-alkyl aldoxime or O-alkyl ketoxime and subsequently separating the N,O-dialkylhydroxylamine hydrochloride from the reaction system; and a process for separating N,O-dialkylhydroxylamine hydrochloride which comprises (i) adding benzene or alkylated benzene to an aqueous solution containing N,O-dialkylhydroxylamine hydrochloride, azeotropically removing water or a hydrochloride solution, and, subsequently (ii)adding alcohol thereto to obtain N,O-dialkylhydroxylamine hydrochloride in the form of crystal.

    摘要翻译： 一种制备N，O-二烷基羟基氨基甲酸酯的方法，其包括使羟胺或其盐与二烃基碳酸酯在碱性化合物的存在下反应以制备羟基氨基甲酸酯，随后用烷基化剂烷基化该化合物; 一种回收N，O-二烷基羟基氨基甲酸酯的方法，该方法包括从含有酯的溶液中用水共沸蒸馏该酯; 一种制备N，O-二烷基羟胺的方法，其包括在碱存在下水溶液或含水溶剂中N，O-二烷基羟基氨基甲酸酯水解; 一种纯化N，O-二烷基羟胺盐酸盐的方法，其包括将醛或酮加入到含有O-烷基羟胺盐酸盐的N，O-二烷基羟胺盐酸盐的溶液中作为杂质，以将O-烷基羟胺盐酸盐转化为O-烷基羟基肟或O-烷基酮肟 随后从反应体系中分离出N，O-二烷基羟胺盐酸盐; 以及分离N，O-二烷基羟胺盐酸盐的方法，其包括（i）将苯或烷基化苯加入到含有N，O-二烷基羟胺盐酸盐的水溶液中，共沸除去水或盐酸盐溶液，随后（ii）向其中加入醇 得到晶体形式的N，O-二烷基羟胺盐酸盐。