反-4-(反-4-正丙基环己基)-环己基丙醛的合成  

SYNTHESIS OF trans-4-(trans-4-PROPYLCYCLOHEXYL)CYCLOHEXYL PROPIONALDEHYDE

作　　者：高丰琴[1] 何汉江 郭强 王小明 何勇 

机构地区：[1]咸阳师范学院化学与化工学院,陕西咸阳712000 [2]西安瑞联近代电子材料有限责任公司,陕西西安710075

出　　处：《精细石油化工》2013年第4期25-29,共5页Speciality Petrochemicals

摘　　要：以反-4-(反-4-正丙基环己基)-环己基甲醛为原料,经Wittig、加氢、酸解反应合成反-4-(反-4-正丙基环己基)-环己基丙醛,总收率71.5%。目标化合物经1 H NMR、13 C NMR、IR和GC-MS表征。探讨了加氢的机理及反应的最佳条件,加氢实验结果表明:以Raney-Ni/MgSO4为催化剂,甲苯乙醇为反应溶剂,当反应温度为35℃,压力为0.5MPa时,反应效果最佳。加氢后粗产物经甲苯甲醇重结晶后用无水甲酸重复酸解两次,原料能酸解至0.01%以下。该合成路线中加氢及酸解反应的突破,推广了反-4-(反-4-正丙基环己基)-环己基丙醛在双环己基液晶单体合成领域中的广泛应用。trans-4-（trans-4-Propylcyclohexyl）cyclohexyl propionaldehyde was synthesized fromtrans4-（trans-4-propylcyclohexyl）cyclohexyl aldehyde via Wittig,hydrogenation and acidolysis reaction with total yield of 71.5%.The target compound was characterized by 1 H NMR,13C NMR,IR and GC-MS.The mechanism and the best reaction conditions of hydrogenation were investigated and the results of condition experiments showed that the reaction effect was best at 35℃under 0.5MPa with Raney-Ni/MgSO4as catalyst,toluene and ethanol as reaction solvent.After hydrogenation,the crude product was recrystallized with toluene and methanol and reacted twice with anhydrous formic acid through acidolysis reaction.the material can be reacted below 0.01%.

关 键 词：反-4-(反-4-正丙基环己基)-环己基丙醛 WITTIG反应 加氢 酸解 合成 

分 类 号：TQ234.1[化学工程—有机化工]