Fractionation of woody biomass with boiling aqueous acetic acid containing a small amount of mineral acid at atmospheric pressure: Reactivity of arylglycerol-β-aryl ethers in lignins with aqueous acetic acid containing H2SO4
Fractionation of woody biomass with boiling aqueous acetic acid containing a small amount of mineral acid at atmospheric pressure: Reactivity of arylglycerol-β-aryl ethers in lignins with aqueous acetic acid containing H2SO4
复制标题
在常压下用含有少量无机酸的沸腾乙酸水溶液对木质生物质进行分馏：木质素中的芳基甘油-β-芳基醚与含有 H2SO4 的乙酸水溶液的反应性
DOI：
10.1007/bf00521966
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发表时间：
1998
影响因子：
2.9
通讯作者：
H. Konno
中科院分区：
文献类型：
--
作者：
Y. Sano;S. Shimamoto;M. Enoki;H. Konno
为了研究木质素与含少量H_2SO_4的醋酸水溶液(AW)的反应机理，将愈创木基甘油-β-愈创木基醚(GOG)和愈创木基甘油-β-丁香醚(GOS)分别在90%AW和0.28%H_2SO_4溶液中回流0~120min。用气相色谱-质谱法和核磁共振等分析方法对反应产物及其硅烷化衍生物进行了表征。当模型化合物在沸腾温度下反应0min(升温时间30min)时，它们的大部分伯醇基团和部分仲醇基团发生乙酰化，而酚基不发生乙酰化。大约90%的GOG在至少15分钟的沸腾过程中被降解、聚合或两者兼而有之，生成愈创木酚和异香豆素化合物(GOG-e和GOG-f)，此外还生成高香草醛(II)作为愈创木基乙烯醇(I)和其他次要产物。GOS得到了辛氨酚、高香草素(II)和一种新化合物(V)以及未知产物，但没有相应的异香豆素化合物。
To characterize the mechanism of the reaction of lignin with aqueous acetic acid (AW) containing a small amount of H2SO4, guaiacylglycerol-β-guaiacyl ether (GOG), and guaiacylglycerol-β-syringol ether (GOS) were refluxed in 90% AW with 0.28% H2SO4 for 0–120 min. Reaction products and their silylated derivatives were characterized by analytical methods such as gas chromatography-mass spectrometry and nuclear magnetic resonance. When the model compounds were allowed to react at boiling temperature for 0 min (heat-up time 30 min), most of their primary alcohol groups and some of their secondary alcohol groups were acetylated, but their phenolic groups were not. About 90% of GOG was degraded, polymerized, or both during boiling for at least 15 min, yielding guaiacol and isocoumaran compounds (GOG-e and GOG-f) in addition to homovanillin (II) as guaiacylvinyl alcohol (I) and other minor products. GOS yielded syringol, homovanillin (II), and a novel compound (V) together with unknown products but not the corresponding isocoumaran compounds.