| 在常压和加压条件下直接合成萜烯马来酸二甲酯加合物 |
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| 引用本文： | 黄坤,唐小东,李梅,连建伟,夏建陵.在常压和加压条件下直接合成萜烯马来酸二甲酯加合物[J].林产化学与工业,2012,32(2):92-96. |
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| 作者姓名： | 黄坤 唐小东 李梅 连建伟 夏建陵 |
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| 作者单位： | 1. 中国林业科学研究院 林产化学工业研究所;生物质化学利用国家工程实验室;国家林业局 林产化学工程重点开放性实验室;江苏省 生物质能源与材料重点实验室, 江苏 南京 210042;;2. 中国林业科学研究院 林业新技术研究所, 北京 100091 |
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| 基金项目： | 国家林业局林业公益性行业科研专项(201104031) |
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| 摘 要： | 以工业双戊烯为原料,马来酸二甲酯为双烯加成试剂,在常压和加压两种条件下合成了萜烯马来酸二甲酯加合物。常压下,加热至185℃回流10 h,产率为55%;压力反应釜中,压力为1.5 MPa,反应温度为240℃,反应2 h即可进行完全,产率为78.6%。纯化产物用GC-MS、1H NMR和FT-IR进行了表征。GC-MS表明经蒸馏纯化的产物中分子离子峰质荷比为280.1的萜烯马来酸二甲酯同分异构体约有20个,纯度为95.2%。经产物的1H NMR计算得到产物中Diels-Alder加成物质量分数为35%。
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| 关 键 词： | 萜烯马来酸二甲酯 双戊烯 Diels-Alder反应 |
Synthesis of Terpene-dimethyl Maleate Adduct under Atmospheric and Pressurized Conditions |
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| HUANG Kun,TANG Xiao-dong,LI Mei,LIAN Jian-wei,XIA Jian-ling.Synthesis of Terpene-dimethyl Maleate Adduct under Atmospheric and Pressurized Conditions[J].Chemistry & Industry of Forest Products,2012,32(2):92-96. |
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| Authors: | HUANG Kun TANG Xiao-dong LI Mei LIAN Jian-wei XIA Jian-ling |
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| Institution: | 1,2(1.Institute of Chemical Industry of Forestry Products,CAF;National Engineering Lab.for Biomass Chemical Utilization; Key and Lab.of Forest Chemical Engineering,SFA;Key Lab.of Biomass Energy and Material,Jiangsu Province, Nanjing 210042,China;2.Institute of New Technology of Forestry,CAF,Beijing 100091,China) |
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| Abstract: | Terpene-dimethyl maleate adduct was prepared under atmospheric and pressurized conditions from industrial dipentene and dimethyl maleate as a dienophile.Under atmospheric condition,the yield of terpene-dimethyl maleate adduct was 55% after reflux at 185 ℃ for 10 h.In the hermetic autoclave,the yield of terpene-dimethyl maleate adduct achieved at 78.6 % after 2 h at 240 ℃ and 1.5 MPa.The adduct was characterized by GC-MS,1 H NMR and FT-IR.GC-MS indicated that there were 20 geometric isomers.The mass charge ratio of those molecular ion peaks was 280.1 in the purified adduct and the purity was 95.2%.The content of the Diels-Alder adduct was about 35% of the purified adduct which was calculated from 1 H NMR. |
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| Keywords: | dimethyl terpene-maleate dipentene Diels-Alder reaction |
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