2-异丙基-1,3-二氧-5-环庚烯的合成及其分析

Synthesis and Analysis of 2-iso-Propyl-1,3-Dioxy-5-Cycloheptene

以对甲苯磺酸为催化剂,通过顺丁烯二醇与异丁醛之间的醛醇缩合反应合成了2-异丙基-1,3-二氧-5-环庚烯,反应温度控制在110~120℃之间,反应时间为5 h。试验求得反应物(顺丁烯二醇与异丁醛)的最佳摩尔比为1比1.2。用带有强极性毛细管色谱柱(60 m×0.25 mm)的气相色谱法测定了反应混合物中2-异丙基-1,3-二氧-5-环庚烯的含量,测定结果表明此产物的质量分数大于98%。应用卡尔-菲休滴定法测定了所合成的产物中的水分,所得结果表明水分的质量分数均小于0.1%。

2-iso-Propyl-1,3-dioxy-5-cycloheptene was prepared by the aldol reaction between cis-butene glycol and iso-butyl aldehyde,with p-toluene sulfonic acid as catalyst,under the reaction temperature of 110-120 ℃ for 5 h.The optimum mole ratio of the reactants was found to be 1 to 1.2 for cis-butene glycol to iso-butyl aldehyde.Gas chromatography with the strongly polar capillary column(60 m×0.25 mm) was used for the determination of 2-iso-propyl-1,3-dioxy-5-cycloheptene in the reaction mixture,giving results of ...