以异长叶烷酮为原料,与水合肼合成异长叶烷基席夫碱,采用单因试验和正交试验考察了不同条件对反应的影响。结果表明,以异长叶烷基席夫碱的得率为考察指标,其合成的最佳工艺条件为:以无水乙醇为反应溶剂,催化剂浓硫酸的用量0.6%(以总物料的体积为基准),反应温度78℃,反应时间24 h,n(异长叶烷酮)∶n(水合肼)为1∶5,此条件下的得率为87.84%。采用GC-MS、FT-IR和1H NMR等手段对所得产物进行了分析与表征,证明合成了异长叶烷基席夫碱。
Isolongifolane ketone Schiff base was synthesized with isolongifolane ketone and hydrazine as raw materials. The effects of different conditions on the reaction were studied by single factor and orthogonal experiments with the yield of the isolongifolane ketone Schiff base as the investigation index. The results showed that the optimized technological parameters were the catalyst dosage 0. 6%( use the volume of all the material as the reference),ethanol as the solvent,reaction time 24 h,reaction temperature 78 ℃ and n( isolongifolane ketone) ∶ n( hydrazine) 1 ∶ 5. Under these conditions,the yield of the product was87. 84%,and its chemical structure was analyzed by GC-MS,FT-IR and ~1H NMR spectra. They proved that the isolongifolane ketone Schiff base was synthesized.