摘要
以罗汉柏木烯为原料,KMnO_(4)为氧化剂,叔丁醇/水(体积比2∶1)为溶剂,通过罗汉柏木烯的双羟基化反应合成得到了罗汉柏木二醇。考察了反应条件对双羟基化反应的影响,得到最佳工艺条件为:反应温度40℃,n(KMnO_(4))∶n(罗汉柏木烯)=1.8∶1,反应时间3 h,KMnO_(4)水溶液质量分数为5%。在此条件下,罗汉柏木烯的转化率为98.3%,罗汉柏木二醇的收率和选择性分别为88.7%和90.2%。采用GC-MS、FT-IR和^(1)H NMR等方法对产物结构进行了表征,确定产物为罗汉柏木二醇。
Thujopsane-8,9-diol was synthesized by the dihydroxylation of thujopsene using KMnO_(4)as oxidant,tertiary-butyl alcohol/H_(2)O(2∶1,volume ratio)as solvent in the presence of NaOH.The effects of reaction conditions on the dihydroxylation reaction were investigated and the optimal reaction conditions were reaction temperature 40℃,molar ratio of raw materials n(KMnO_(4))∶n(thujopsene)=1.8∶1,reaction time 3 h,mass fraction of KMnO_(4) aqueous solution 5%.Under these conditions,the conversion rate of thujopsene was 98.3%,the yield and selectivity of thujopsane-8,9-diol were 88.7%and 90.2%,respectively.The structure of the product was characterized by GC-MS,FT-IR and ^(1)H NMR,and confirmed to be thujopsane-8,9-diol.
作者
张胜
朱凯
毛萍
ZHANG Sheng;ZHU Kai;MAO Ping(College of Chemical Engineering,Nanjing Forestry University,Nanjing 210037,China;Co-Innovation Center of Efficient Processing and Utilization of Forest Resources,Nanjing Forestry University,Nanjing 210037,China;Nanjing Eurasia Flavors&Fragrances Co.,Ltd.,Nanjing 210037,China)
出处
《林产化学与工业》
CAS
CSCD
北大核心
2022年第2期110-114,共5页
Chemistry and Industry of Forest Products
基金
国家重点研发计划资助项目(2018YFD0600405)
江苏高校优势学科建设工程项目(无编号)。