正交试验法优化合成环己酮Vc缩酮  

Optimized synthesis of cyclohexanone L-ascorbic acid ketal by orthogonal experiment

作　　者：郑大贵[1] 余衍文[2] 

机构地区：[1]上饶师范学院,江西省普通高校应用有机化学重点实验室,江西上饶334001 [2]南昌大学化学系,江西南昌330031

出　　处：《化学研究与应用》2008年第11期1487-1490,共4页Chemical Research and Application

基　　金：江西省普通高校重点实验室科技计划项目(赣教技字[2006]302号)资助

摘　　要：Cyclohexanone L-ascorbic acid ketal is synthesized from the reaction of L-isoascorbic acid and cyclohexanone with p-toluene sulfonic acid as catalyst,N,N-dimethyl acetamide(DMAc) as solvent and cyclohexane as water carrying agent.The optimal reaction conditions determined by orthogonal experiment are as follows:L-ascorbic acid 1.76 g(10 mmol),cyclohexanone 1.57 g(16 mmol),p-toluene sulfonic acid 0.38 g(2 mmol),DMAc 6 mL,cyclohexane 9 mL,reaction temperature 120～125℃ and reation time 2.5 h.The yield is 85.8% under these optimal conditions.The title compound is characterized by 1H NMR,FTIR and EI-MS.Cyclohexanone L-ascorbic acid ketal is synthesized from the reaction of L-isoascorbic acid and cyclohexanone with ptoluene sulfonic acid as eatalyst,N,N-dimethyl acetamide（DMAe） as solvent and cyclohexane as water carrying agent. The optimal reaction conditions determined by orthogonal experiment are as follows ：L-ascorbic acid 1.76 g（ 10 mmol）, eyclohexanone 1.57 g （16 retool）,p-toluene sulfonic acid 0. 38 g（2 mmol）, DMAc 6 mL, eyelohexane 9 mL, reaction temperature 120 ～ 125℃ and reation time 2. 5 h. The yield is 85.8% under these optimal conditions. The title compound is characterized by ^1H NMR, FTIR and EI-MS.

关 键 词：环己酮Vc缩酮 环己酮 VC 对甲苯磺酸 正交试验 

分 类 号：O621.256.4[理学—有机化学]