亚磷酸三(1-环己氧基-2,2,6,6-四甲基哌啶基)酯的合成及表征

Synthesis and Characterization of Tris(1-cyclohexyloxy-2,2,6,6-tetramethyl piperidine-4-yl)phosphite

对以1-环己氧基-4-羟基-2,2,6,6-四甲基哌啶醇(简称CHPOL)和三氯化磷为原料,合成亚磷酸三(1-环己氧基-2,2,6,6-四甲基哌啶基)酯进行了研究,并通过IR、~1H NMR、^(13)C NMR和^(31)P NMR表征了其结构。其较佳的合成工艺条件是:氯仿为溶剂,三乙胺为缚酸剂,n(PCl3)∶n(CPOL)∶n(三乙胺)=1∶3∶9,反应时间为8h,反应温度为30℃。在此条件下,产品的摩尔分数为98.04%,磷收率为68.57%。

Tris(1-cyclohexyloxy-2,2,6,6-tetramethyl piperidine-4-yl)phosphite was synthesized by using 1-cyclohexyloxy-2,2,6,6-tetramethylpiperidine-4-ol(referred as CHPOL)and phosphorus trichloride as raw materials,and its structure was characterized by IR,1H NMR,13 C NMR and 31 P NMR.The results revealed that the optimal conditions were:Chloroform as solvent,triethylamine as acid-binding agent,n(PCl 3)∶n(CHPOL)∶n(triethylamine)=1∶3∶9,the reaction time being 8 h,and the reaction temperature being 30℃.Under the above conditions,the molar content of the products was 98.04%and the yield of phosphorus was 68.57%.