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    • 2. 发明授权
    • Preparation of n-methoxy-n-methylurethanes
    • 正 - 甲氧基 - 正 - 甲基氨基甲酸酯的制备
    • US4469884A
    • 1984-09-04
    • US484886
    • 1983-04-14
    • Gernot ReissenweberUlrich Schirmer
    • Gernot ReissenweberUlrich Schirmer
    • C07C271/08C07C67/00C07C239/00C07C271/06C07C125/065
    • C07C271/06
    • N-Methoxy-N-methylurethanes are prepared by a process in which first (1) hydroxylamine is converted with an alkyl chloroformate to the corresponding N-hydroxyurethane, then (2) this product is reacted with a methylating agent to give the N-methoxy-N-methylurethane, and finally (3) the N-methoxy-N-methylurethane is isolated. In this process, first, (1) while maintaining a certain temperature and a certain pH, (1.1) an aqueous solution of an inorganic hydroxylammonium salt is mixed thoroughly with (1.2) an equimolar amount of an alkyl chloroformate, then (2) while maintaining a certain temperature and a certain pH, (2.1) a mixture comprising (2.1.1) the reaction mixture obtained as described in (1), (2.1.2) a water-insoluble organic solvent and (2.1.3) a phase-transfer catalyst is mixed thoroughly with (2.2) a water-insoluble methylating agent which is soluble in the solvent under (2.1.2), and the resulting mixture is kept at a certain temperature for a certain time, and finally (3) any methylating agent still present in the reaction mixture obtained as described in (2) is destroyed, the non-aqueous liquid phase is separated off from the mixture thus treated, and the N-methoxy-N-methylurethane is isolated from this phase by stripping off the solvent. A relatively pure product is obtained in high yield.
    • N-甲氧基-N-甲基氨基甲酸酯通过以下方法制备:首先(1)羟胺用氯甲酸烷基酯转化为相应的N-羟基氨基甲酸酯,然后(2)将该产物与甲基化剂反应,得到N-甲氧基 -N-甲基氨基甲酸酯,最后(3)分离出N-甲氧基-N-甲基氨基甲酸酯。 在此过程中,首先,(1)在保持一定温度和一定pH值的情况下,(1.1)将无机羟基铵盐的水溶液与(1.2)等摩尔量的氯甲酸烷基酯充分混合,然后(2)同时 保持一定的温度和一定的pH,(2.1)一种混合物,其包含(2.1.1)如(1),(2.1.2)中所述获得的反应混合物为水不溶性有机溶剂和(2.1.3)相 转移催化剂与(2.2)一种水溶性甲基化剂(2.2)溶于(2.1.2)溶剂中,将所得混合物在一定温度下保持一定时间,最后(3)任何 如(2)所述的反应混合物中仍然存在的甲基化剂被破坏,将非水性液相与被处理的混合物分离,通过剥离从该相中分离出N-甲氧基-N-甲基氨基甲酸酯 溶剂。 以高产率获得相对纯的产物。