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[1]游华彬,潘志权*,周红.三氯蔗糖6乙酯的制备工艺[J].武汉工程大学学报,2011,(04):26-29.[doi:10.3969/j.issn.16742869.2011.04.007]
　YOU Hua bin,PAN Zhi quan,ZHOU Hong.Study on chlorination of sucrose6acetate[J].Journal of Wuhan Institute of Technology,2011,(04):26-29.[doi:10.3969/j.issn.16742869.2011.04.007]
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三氯蔗糖6乙酯的制备工艺(/HTML)
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《武汉工程大学学报》[ISSN:1674-2869/CN:42-1779/TQ]

卷:
期数:
2011年04期
页码:
26-29
栏目:
化学与化学工程
出版日期:
2011-04-30

文章信息/Info

Title:
Study on chlorination of sucrose6acetate
文章编号:
16742869(2011)04002604
作者:
游华彬; 潘志权*; 周红
武汉工程大学,绿色化工过程省部共建教育部重点实验室,湖北 武汉 430074
Author(s):
YOU Huabin;  PAN Zhiquan;  ZHOU Hong
Key Laboratory for Green Chemical Process of Ministry of Education,
School of Chemical Engineering and Pharmacy, Wuhan Institute of Technology, Wuhan 430074, China
关键词:
三氯蔗糖6乙酯; Vilsmeier试剂; 工艺优化
Keywords:
sucralose6acetate;  vilsmeier reagent;  process optimization
分类号:
TS201.2
DOI:
10.3969/j.issn.16742869.2011.04.007
文献标志码:
A
摘要:
以蔗糖为原料,经选择性酯化,SOCl2和DMF原位制备的Vilsmeier试剂氯化制备了三氯蔗糖6乙酯,并经IR、1H NMR确认其结构;考察了投料顺序对氯化收率的影响,实验表明事先制备Vilsmeier试剂利于提高氯化收率;研究了二氯取代反应温度和反应时间对氯代反应的影响,发现在98~100 ℃反应6 h,二氯取代基本完成;同时也研究了氯化液的后处理方法,以二氯甲烷洗涤水相,再经萃取,乙酸乙酯水结晶,使两步产率达41%.优化后的氯化工艺简单易控制,利于工业化生产.
Abstract:
Sucrose6acetate was synthesized based on chlorination of vilsmeier reagent by thionyl chloride, which was prepared from sucrose via selective esterification, and the structure was confirmed by IR, 1H NMR；The studies on the process of syntheses show that vilsmeier reagent prepared prior is necessary to increase the yield of chlorination；the most excellent condition for dichlorosubstituted reaction is at 98—100℃ for 6h. Chloride reaction solution was extracted with dichloromethane and then crystallized with ethyl acetatewater in 41% yield. The optimized process of chlorination was simple and more easy to control and suitable for industrial production.

参考文献/References:

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备注/Memo

备注/Memo:
收稿日期：20101109作者简介：游华彬（1983），男，湖北宜昌人，硕士研究生.研究方向：精细化学品的开发.指导教师：潘志权，教授,博士，博士研究生导师.研究方向：配位化学.
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