摘要
以罗汉柏木烯为原料,二氯甲烷为溶剂,甲基三氧化铼(MTO)为催化剂,H_(2)O_(2)为氧化剂,3-甲基吡唑为碱性配体,进行氧化反应合成罗汉柏木烷酮。考察了反应条件对氧化反应的影响,得到最佳工艺条件为:反应温度30℃,n(H_(2)O_(2))∶n(罗汉柏木烯)=2∶1,反应时间3 h,催化剂用量为0.3%(以罗汉柏木烯质量计,下同),3-甲基吡唑用量为10%。在最佳工艺条件下,产物得率为72.1%,罗汉柏木烯转化率为97.3%。采用FT-IR和GC-MS分析方法对产物进行表征,确定产物为罗汉柏木烷酮。
Thujopsanone was synthesized by oxidation reaction with thujopsene as raw material,dichloromethane as solvent,methyltrioxorhenium(MTO)as catalyst,30%H_(2)O_(2) as oxidant,and 3-methylpyrazole as co-catalyst.The effects of reaction conditions on the oxidation were studied.The optimized reaction were obtained as follows:the reaction temperature 30℃,the molar ratio of raw materals(n(H_(2)O_(2))∶n(thujopsene))1∶1,the reaction time 3 h,the catalyst amounts 0.3%(based on the weight of thujopsene,similarly hereinafter),the dosage of 3-methylpyrazole is 10%.Under these conditions,the yield of thujopsanone was 72.1%,and the conversion rate of thujopsene was 97.3%.The structure of the products was identified by GC-MS and FT-IR,and it was confirmed as wasthujopsanone.
作者
张胜
朱凯
ZHANG Sheng;ZHU Kai(College of Chemical Engineering,Nanjing Forestry University,Nanjing 210037,China;Jiangsu Co-Innovation Center of Efficient Processing and Utilization of Forest Resources,Nanjing Forestry University,Nanjing 210037,China)
出处
《林产化学与工业》
CAS
CSCD
北大核心
2021年第4期23-28,共6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)。
