金蕴华, 周子清, 成冰如, 胡漢和. 磷酸胡椒嗪制备方法的研究J. 药学学报, 1963, 10(12): 737-739.
引用本文: 金蕴华, 周子清, 成冰如, 胡漢和. 磷酸胡椒嗪制备方法的研究J. 药学学报, 1963, 10(12): 737-739.
KING YUN-HUA, CHOW TZE-CHIN, CHENG BIN-RU AND HU HAN-HO, . RESEARCH ON THE PREPARATION OF PIPERAZINE PHOSPHATEJ. Acta Pharmaceutica Sinica, 1963, 10(12): 737-739.
Citation: KING YUN-HUA, CHOW TZE-CHIN, CHENG BIN-RU AND HU HAN-HO, . RESEARCH ON THE PREPARATION OF PIPERAZINE PHOSPHATEJ. Acta Pharmaceutica Sinica, 1963, 10(12): 737-739.

磷酸胡椒嗪制备方法的研究

RESEARCH ON THE PREPARATION OF PIPERAZINE PHOSPHATE

  • 摘要: 本文报导利用糖精(甲苯磺酰化法)的副产物对甲苯磺酰氯为原料,先制成对甲苯磺酰胺;然后在碱存在下与二氯乙烷进行缩合生成N,N′-双(对甲苯磺酰)胡椒嗪;再经浓磷酸高温水解成胡椒嗪的酸性磷酸盐;最后经碱中和即得临床上需用的磷酸胡椒嗪一水合物,对于缩合反应的反应时间、配料比例、缩合剂和中和剂的选择,溶剂的影响以及反应后处理的方法等都进行了一些考察.

     

    Abstract: A convenient method is reported for the preparation of piperazine phosphate, an anthelmintie and pharmaceutical intermediate. p-Toluenesulphonyl chloride, a by-product from saccharin manufacture, was first converted into p-toluenesulphonamide which was then condensed with ethylene dichloride in the presence of anhydrous potassium carbonate to form N,N'-bis-(p-toluenesulphonyl)-piperazine. Hydrolysis with concentrated phosphoric acid gave piperazine acid phosphate; the latter on partial neutralization with sodium or calcium hydroxide gave directly the expected' piperazine phosphate monohydrate, m.p. 224—6℃. Experimental conditions were studied.

     

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