一种新型环氧磷酸酯的合成和表征

以氯磷酸二乙酯、3-环己烯-1-甲醇为原料,首先合成3-环己烯-1-甲酯缩磷酸二乙酯(CDP),然后在CDP的基础上合成3-氧化环己烯-1-甲酯缩磷酸二乙酯(OCDP).通过正交实验找出两步反应的较优条件.当反应温度为80℃,n(氯磷酸二乙酯)∶n(3-环己烯-1-甲醇)∶n(三乙胺)=1∶1.5∶1,反应时间为36h时,CDP收率可达80.6%.当反应温度为80℃,n(CDP)∶n(过氧单磺酸钾)∶n(四丁基溴化铵)=1∶2∶1,反应时间为36h时,最终产物OCDP的收率为87.6%.通过红外光谱以及核磁共振分别对两步产物的结构进行表征.

Synthesis and characterization of a new type of epoxy phosphate

Using diethyl chlorophosphate and 3-cyclohexene-1-methanol as initial materials,3-cyclohexene-1-methyl ester diethyl phosphate (CDP) was synthesized on the first step,and the final product 3-cyclohexene oxide-1-methyl ester diethyl phosphate (OCDP) was synthesized on the second step on the base of CDP.The optimum synthesis process was obtained by orthogonal experiment and the results showed that the optimum synthesis process was:for the first step,when reaction temperature was 80 ℃,n (diethyl chlorophosphate):n (3-cyclohexene-1-methanol) ∶ n (triethylamine) was 1 ∶ 1.5 ∶ 1,reaction time was 36 h,the yield was 80.6％;for the second step,when reaction temperature was 80 ℃,n (CDP) ∶ n (potassiumperoxomonosulfate) ∶ n (tetrabutyl ammonium bromide) was 1 ∶ 2 ∶ 1,reaction time was 36 h,the yield was 87.6％.The chemical structure of the products was confirmed by IR and 1H NMR.