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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

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【作者】 郑大贵余衍文

【Author】 ZHENG Da-gui1,YU Yan-wen2(1.Key Laboratory of Applied Organic Chemistry,Higher Institutions of Jiangxi Province,Shangrao Normal College,Shangrao 334001,China;2.Chemistry Department,Nanchang University,Nanchang 330031,China)

【机构】 上饶师范学院,江西省普通高校应用有机化学重点实验室南昌大学化学系

【Abstract】 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.

【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
  • 【文献出处】 化学研究与应用 ,Chemical Research and Application , 编辑部邮箱 ,2008年11期
  • 【分类号】O624.42
  • 【被引频次】4
  • 【下载频次】155
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