笔者以α-蒎烯为原料高选择性环氧化合成2,3-环氧蒎烷。探讨了过氧乙酸浓度及用量、碳酸钠用量、溶剂类型、反应温度及反应时间等对α-蒎烯转化率、2,3-环氧蒎烷选择性及产物组成的影响; 确定了适宜的环氧化反应条件:反应温度为0～10 ℃; 过氧乙酸浓度2.0 mol/L,α-蒎烯与过氧乙酸物质量之比为1:1.1; α-蒎烯与碳酸钠物质量之比为1:1.2; 反应时间2 h; 以氯仿为溶剂,溶剂用量为α-蒎烯与氯仿体积比1:1.7。在此条件下α-蒎烯转化率为99%以上,2,3-环氧蒎烷的选择性大于95%,反应产物中主要杂质α-龙脑烯醛和3-蒎酮的含量仅为3.3%和1.2%左右。
Abstract
2,3-epoxypinane was synthesized from α-pinene by epoxidation with high selectivity. Effects of concentration and dosage of peracetic acid, dosage of anhydrous sodium carbonate, solvent types, reaction temperature and reaction time on the conversion of α-pinene were investigated, respectively. Mean while the selectivity of 2,3-epoxypinane and chemical compositions of the products were investigated too. The most suitable reaction conditions were finally determined as follows: temperature 0-10 ℃, concentration of peracetic acid 2.0 mol/L, molar ratio of α-pinene and peracetic acid 1:1.1,molar ratio of α-pinene and Na2CO3 1:1.2, reaction time 2.0 h, using CHCl3 as the solvent and volume ratio of α-pinene and CHCl3 1:1.7. At this condition, conversion rate of α-pinene was above 99%, selectivity of 2,3-epoxypinane was more than 95%. The contents of the main impurities α-campholenic aldehyde and 3-pinonic in the final product were only 3.3% and 1.2% respectively.
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基金
收稿日期:2012-07-16 修回日期:2012-10-09
基金项目:国家林业公益性行业科研专项项目(201104015); 国家自然科学基金项目(30972316)
第一作者:徐徐,讲师。*通信作者:王石发,教授,博士。E-mail:wsfyyq@njfu.com.cn。
引文格式:徐徐,刘兵,唐年华,等. α-蒎烯高选择性环氧化合成2,3-环氧蒎烷的研究[J]. 南京林业大学学报:自然科学版,2013,37(1):96-100.
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