微波辅助、磷酸催化合成半乳聚糖的结构分析

Preparation and Structural Characterization of Galactans Synthesized by Phosphoric Acid Catalyzation under Microwave Irradiation

DOI：10.3969/j.issn.1673-1689.2017.01.005

中文关键词: 微波 磷酸 半乳聚糖 结构分析

英文关键词: microwave,phosphoric acid,galactan,structural analyses

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中文摘要:

以磷酸催化、微波辅助合成半乳聚糖为研究对象，探讨半乳聚糖的化学结构及聚合反应的区域选择性和立体选择性。综合采用高效凝胶渗透色谱、红外光谱、甲基化分析及一维、二维核磁共振波谱（1H NMR，13C NMR，1H-1H COSY，TOCSY，HSQC，HMBC），对半乳聚糖的相对分子质量、糖苷键的立体构型和连接位点进行表征。结果表明，反应合成的半乳聚糖为多分支结构，重均相对分子质量为2 657，重均聚合度为16，糖残基以?琢-型半乳吡喃糖为主，主要为→4）-?琢-D-Galp（1→和→2，4）-?琢-D-Galp（1→片段。结构分析结果进一步表明，微波辅助、磷酸催化半乳糖缩合过程中，不同位点的羟基具有不同的反应活性，4位羟基的反应活性最强。

英文摘要:

Galactans synthesized by phosphoric acid catalysis and microwave irradiation were studied for their chemical structures and regio- and stereo-selectivities during the polymerization. A series of analyses including high-performance gel-permeation chromatography，infrared spectroscopy，methylation analysis and NMR spectroscopies（1H，13C，1H-1H COSY，TOCSY，HSQC，HMBC） were used. Results showed that the degree of galactosyl polymerization was 16 and the -galactopyranosyl residues were dominant mainly with →4）-?琢-D-Galp（1→ and →2，4）-?琢-D-Galp（1→ fragments. Structural analyses further indicated that the activities of hydroxyls in galactose were different and the 4-OH exhibited the highest potency.

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