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林产化学与工业

林产化学与工业 ›› 2011, Vol. 31 ›› Issue (1): 31-34.

• 研究报告 • 上一篇    下一篇

诺卜醇脱水合成诺卜二烯反应的研究

隋管华, 赵振东, 李冬梅, 毕良武, 王婧, 陈玉湘   

  1. 中国林业科学研究院 林产化学工业研究所;生物质化学利用国家工程实验室;国家林业局 林产化学工程重点开放性实验室;江苏省生物质能源与材料重点实验室, 江苏 南京 210042
  • 收稿日期:2010-04-05 修回日期:1900-01-01 出版日期:2011-02-28 发布日期:2011-02-28
  • 通讯作者: 赵振东,研究员,博士,博士生导师,主要从事萜类天然产物化学利用等方面的研究工作;E-mail:zdzhao@189.cn。

Synthesis of Nopadiene by Dehydration of Nopol

SUI Guan-hua, ZHAO Zhen-dong, LI Dong-mei, BI Liang-wu, WANG Jing, CHEN Yu-xiang   

  1. Institute of Chemical Industry of Forest Products, CAF;National Engineering Lab.for Biomass Chemical Utilization; Key and Open Lab.on Forest Chemical Engineering, SFA;Key Lab.of Biomass Energy and Material, Jiangsu Province, Nanjing 210042, China
  • Received:2010-04-05 Revised:1900-01-01 Online:2011-02-28 Published:2011-02-28

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摘要： 研究了诺卜醇在负载硫酸铜硅胶脱水剂催化作用下脱水制备诺卜二烯的反应,考察和优化了自制脱水剂配方、用量、反应时间及带水剂用量等影响脱水反应的主要因素。优化的脱水反应条件为:硫酸铜与诺卜醇的物质的量之比为1:4,催化剂中硅胶与硫酸铜的质量比为4:1,反应时间4h,甲苯作为溶剂兼带水剂(用量为诺卜醇质量的14倍)。优化条件下诺卜二烯收率为83.0%,GC含量为91.0%。经过FT-IR、GC-MS和1HNMR等分析鉴定了诺卜二烯的化学结构,初步探讨了反应机理。

关键词: 诺卜二烯, 诺卜醇, 硫酸铜, 硅胶负载硫酸铜

Abstract: The copper sulfate-loaded on silica gel was used as a catalytic agent for the dehydration of nopol to prepare nopadiene. Major factors influencing the reaction, such as the composition of the copper sulfate-loaded silica-gel, dosage of the dehydrating agent to nopol, reaction time and amount of water-carrying solvent, were investigated and optimized in detail. Under the optimum reaction conditions, i.e the mass ratio of silica gel to copper sulfate 4:1, the molar ratio of copper sulfate in the dehydrating agent to nopol 1:4, reaction time 4h, and using toluene as a water-carrying solvent (14 times to nopol in mass), nopadiene was prepared at a yield of 83.0% with a GC purity of 91.0%. The structure of nopadiene was characterized and identified by FT-IR, GC-MS and 1HNMR. The reaction mechanism was also proposed.

Key words: nopadiene, nopol, copper-sulfate-loaded silica-gel

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