摘要
为了克服D-甘露糖植物提取法易破坏资源,钼酸催化化学制备成本高昂,硅醚保护羟基过程步骤繁琐的缺点,本论文以羟基都没有保护的D-甘露醇为原料,利用FeCl_(2)/H_(2)O_(2)的水相体系直接催化末端羟基一步氧化并脱去一分子水形成目标产物D-甘露糖。考察了时间,pH值,温度,双氧水的加入体积和氯化亚铁的加入量对生成D-甘露糖的影响,分析讨论了以上5个因素对D-甘露糖催化合成产率的影响,并且将反应投料量放大到公斤级,在最优反应条件下平行三批次的产率达到27.02±0.81%,并通过红外,核磁,高分辨的初步结构表征,确证了最终的目标产物是D-甘露糖。
In this study,a convenient,low-cost,environmentally friendly,and scalable synthesis method for D-mannose was development.It presented a method for preparing the target product by using FeCl_(2)/H_(2)O_(2)aqueous system to directly catalyze oxidation in one step.The effects of time,pH value,temperature,volume of hydrogen peroxide,and amount of ferrous chloride on the yield of Dmannose were investigated in the one single-factor experiment.Under optimal reaction conditions,the yield reached to 27.02±0.81%(n=3)in kilogram grade reactional raw materials.Meanwhile,the structure of D-mannose was further confirmed by IR,nuclear magnetic resonance,and high-resolution structural.
作者
方华
黄梦贤
陈伟珠
石国宗
晋文慧
陈晖
张怡评
FANG Hua;HUANG Meng-xian;CHEN Wei-zhu;SHI Guo-zong;Jin Wen-hui;CHEN Hui;ZHANG Yi-ping(Technical Innovation Center for Utilization of Marine Biological Resources,Third Institute of Oceanography,Ministry of Natural Resources,Xiamen 361005,China;School of Marine Biology,Xiamen Ocean Vocational College,Xiamen 361102,China;College of Biology and Environment,Zhejiang Wanli University,Ningbo 315100,China)
出处
《化学研究与应用》
北大核心
2025年第12期3831-3835,共5页
Chemical Research and Application
基金
福建省科技厅专项资金项目(2024Y0078)资助
厦门海洋与渔业局专项资金项目(23CZP009HJ11)资助。
关键词
甘露糖
催化合成
水相体系
单因素实验
D-mannose
catalytic synthesis
aqueous system
single factor experiment
