3,3’-二甲基(对双胍基)二环己基甲烷的合成及表征

Synthesis and Characterization of 3,3'-dimethyl (P-guanidino) Dicyclohexylmethane

以双氰胺和3,3’-二甲基-4,4’-二氨基二环己基甲烷(DMDC)为原料,在酸性条件下进行加成反应,经分离提纯并干燥得到白色颗粒状固体产物,并通过红外光谱谱图和核磁图谱对产物进行表征,表明产物为3,3’-二甲基(对双胍基)二环己基甲烷(DGDM)。通过设计正交试验对反应条件进行优化,实验结果表明:反应温度140℃,反应时间9h,n(DMDC):n(双氰胺)=1:2.1,反应产率最高为81.3%。

The addition reaction was carried out under the acidic conditions using dicyandiamide and 3,3＇-dimethyl-4,4＇-diaminodicyclohexylmethane（DMDC） as raw materials to prepare 3,3＇-dimethyl（Pguanidino） dicyclohexylmethane. The effects of reaction temperature, reaction time and molar ratio of materials on the yield of the product were discussed. The products were characterized by IR spectra and NMR spectra. The results showed that the optimum reaction conditions were as follows： reaction temperature 130 °C, reaction time 9 h, the optimum acidity is concentrated hydrochloric acid in an amount of 1 ∶1.1, n（DMDC）∶n（Dicyandiamide） = 1∶2. Under these conditions, the yield of crude product was 81.3%.