氯代磷酸双(2,4-二氯苯基)酯的合成

以2,4-二氯苯酚和三氯氧磷为原料,在无水氯化铝催化下,合成了氯代磷酸双(2,4-二氯苯基)酯。用正交实验法得到了优化工艺条件:n(2,4-二氯苯酚)∶n(三氯氧磷)=1.7∶1、催化剂用量0.64%、第一段反应温度120℃反应时间2h、第二段反应温度150℃反应时间3h,收率约85.5%。较文献报道,反应时间从34h缩短至5h。产物结构经核磁共振、红外光谱对产物进行了表征。

STUDY ON THE SYNTHESIS OF BIS(2,4-DICHLOROPHENYL) CHLOROPHOSPHATE

Bis(2,4-dichlorophenyl) chlorophosphate was synthesized by the reaction of 2,4-dichloride and phosphorus with aluminium chloride as catalyst.The reaction conditions including the amount of catalyst,the amount of raw materials,reaction temperature and reaction time were studied in detail by the orthogonally arranged experiments.Under the optimized conditions,the total yield reached 85.5%.Compared with the reported results in the literature,the reaction time was reduced from 34 h to 5 h.The product was characterized by 1H NMR,IR.