异长叶烯酮的绿色合成研究

摘要

Isolongifolenone was synthesized by using heavy turpentine as the starting material. Firstly, the heavy turpentine was converted to isolongifolene by isomerization reaction with BF3 ( C2 H5 ) 2 O as catalyst. Isolongifolenone was finally obtained from isolongifolene by allylic oxidation with tert-butyl hydroperoxide ( TBHP) as oxidizer,Cu as catalyst and tert-butyl alcohol ( TBA) as solvent. By investigating the influence of different react conditions on the oxidation of isolongifolene,the optimum conditions were determined as follows:the mass fraction of Cu 3% ( based on the mass of isolongifolene ) , the mole ratio of TBHP and isolongifolene 3. 5∶1,the mass ratio of TBA and isolongifolene 1∶1,reaction temperature 80 ℃ and reaction time 12 h. The yield of isofolenone was over 93%,and the purity was 98. 75% under these conditions.%以重质松节油为原料,经三氟化硼乙醚催化异构得到异长叶烯；采用Cu为催化剂、叔丁基过氧化氢( TBHP)为氧化剂、叔丁醇( TBA)为溶剂经烯丙位氧化得到异长叶烯酮。探讨了反应条件对异长叶烯氧化反应的影响,确定了适宜的氧化工艺条件为：Cu粉用量3%(以异长叶烯质量计),TBHP与异长叶烯物质的量比3.5∶1,溶剂TBA与异长叶烯的质量比1∶1,80℃温度下反应12 h,在此工艺条件下,异长叶烯酮得率达93%,纯度98.75%。