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    • 7. 发明公开
    • VERFAHREN ZUR HERSTELLUNG VON HYDROXYALKANCARBONSÄUREAMIDEN
    • VERFAHREN ZUR HERSTELLUNG VONHYDROXYALKANCARBONSÄULAMIDEN
    • EP0639177A1
    • 1995-02-22
    • EP93911742.0
    • 1993-05-05
    • SCHERING AKTIENGESELLSCHAFT
    • SCHOLZ, StefanHARRE, MichaelVIDIC, Hans-JörgNEEF, GünterKIRSCH, Gerald
    • C07C231C07C235C07D295
    • C07D295/182C07C231/02
    • The description relates to a process for producing hydroxyalkane carboxylic acid amides of the general formula (I), in which n is a whole number from 1 to 20 and R1 and R2 are alkyl groups with a maximum of 8 carbon atoms or together represent an alkylene group with 4 to 8 carbon atoms, possibly interrupted by an oxygen or a nitrogen atom, from hydroxyalkane carboxylic acids of the general formula (II): HO-CnH2n-COOH, in which n has the significance given above and amines of the general formula (III), in which R1 and R2 have the significance given above, characterized in that the hydroxylalkane carboxylic acid is heated with reflux in a one-pot reaction with 10 to 30 mol acetyl chloride per mol acid, the superfluous acetyl chloride is distilled off after acetylisation, the residue is heated with reflux with 1.5 to 5 mol thionyl chloride per mol acid, after the formation of acid chloride the thionyl chloride is distilled off, the residue is dissolved in a dialkyl ether with 4 to 8 carbon atoms, the solution obtained is added proportionately to an aqueous solution of the amine cooled to 0 to 10 °C and, after amide formation, the acetal group is separated off by treatment with aqueous sodium hydroxide solution at a reaction temperature of 10 to 30 °C.
    • 描述涉及通式(I)的羟基链烷羧酸酰胺的制备方法,其中n是1至20的整数,并且R 1和R 2是具有最多8个碳原子的烷基或共同表示亚烷基 (II)的羟基烷烃羧酸与可能被氧或氮原子间隔的具有4至8个碳原子的基团:HO-C n H 2n -COOH,其中n具有上面给出的含义,以及通式 (III)的化合物,其中R1和R2具有上面给出的含义,其特征在于羟基链烷羧酸在回流条件下与每摩尔10-30摩尔乙酰氯在一锅反应中加热,蒸除多余的乙酰氯 在乙酰化之后,将残余物与每摩尔1.5-5摩尔亚硫酰氯加热回流,形成酰氯之后,蒸出亚硫酰氯,将残余物溶于含有4-8碳的二烷基醚 n原子时,将所得溶液按比例加入冷​​却至0-10℃的胺水溶液中,酰胺形成后,在10-30℃的反应温度下用氢氧化钠水溶液处理分离出缩醛基 C。