诺卜醇脱水合成诺卜二烯反应的研究

Synthesis of Nopadiene by Dehydration of Nopol

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4 h,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1H NMR等分析鉴定了诺卜二烯的化学结构,初步探讨了反应机理。

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 4 h, 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 FF-IR, GC-MS and ^1H NMR. The reaction mechanism was also proposed.