林产化学与工业
林產化學與工業
림산화학여공업
CHEMISTRY AND INDUSTRY OF FOREST PRODUCTS
2015年
3期
97-103
,共7页
彭晗%杨丽娟%徐徐%王石发
彭晗%楊麗娟%徐徐%王石髮
팽함%양려연%서서%왕석발
重质松节油%异长叶烯%烯丙位氧化%异长叶烯酮
重質鬆節油%異長葉烯%烯丙位氧化%異長葉烯酮
중질송절유%이장협희%희병위양화%이장협희동
heavy turpentine%isolongifolene%allylic oxidation%isolongifolenone
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%。
以重質鬆節油為原料,經三氟化硼乙醚催化異構得到異長葉烯;採用Cu為催化劑、叔丁基過氧化氫( TBHP)為氧化劑、叔丁醇( TBA)為溶劑經烯丙位氧化得到異長葉烯酮。探討瞭反應條件對異長葉烯氧化反應的影響,確定瞭適宜的氧化工藝條件為:Cu粉用量3%(以異長葉烯質量計),TBHP與異長葉烯物質的量比3.5∶1,溶劑TBA與異長葉烯的質量比1∶1,80℃溫度下反應12 h,在此工藝條件下,異長葉烯酮得率達93%,純度98.75%。
이중질송절유위원료,경삼불화붕을미최화이구득도이장협희;채용Cu위최화제、숙정기과양화경( TBHP)위양화제、숙정순( TBA)위용제경희병위양화득도이장협희동。탐토료반응조건대이장협희양화반응적영향,학정료괄의적양화공예조건위:Cu분용량3%(이이장협희질량계),TBHP여이장협희물질적량비3.5∶1,용제TBA여이장협희적질량비1∶1,80℃온도하반응12 h,재차공예조건하,이장협희동득솔체93%,순도98.75%。
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.