微波辐射下酰基化反应研究.pdf

河北大学
硕士学位论文
微波辐射下酰基化反应的研究
姓名:李红亚
申请学位级别:硕士
专业:有机化学
指导教师:李慧章;李记太
20040601
摘要
摘要

本文分为四部分:
第一部分微波辐射用于有机合成的技术越来越受到了人们的重视微波加
热能提高反应速率数百倍乃至上千倍且具有操作方便副产物少产率很高
产物易纯化等优点本文就近几年来微波技术在有机合成中的应用作一综述
第二部分本文描述了在甲酸既为溶剂又为甲酰化试剂条件下通过微波辐
射合成 N-芳基甲酰胺的实验过程利用熔点及红外光谱对产物的结构进行了鉴
定与经典方法相比产率有所提高反应时间缩短了 20-120 倍
第三部分以硫酚及氯丙酸为原料在微波辐射和水溶剂的条件下合成了
系列的芳硫丙酸并进一步以芳硫丙酸为原料在微波辐射及多聚磷酸的作用下
脱水关环合成了抗菌剂硫色满酮与经典方法相比反应时间大大缩短产率有
所提高而且操作大为简化
第四部分以芳氧乙酸芳硫乙酸为原料探讨了使用硅胶固载氯磺酸催
化剂催化的酯化反应并用核磁共振对所得产物进行表征通过与经典方法进行
比较结果表明实验处理简单催化剂可回收对环境污染小该方法反应时
间短产率高

关键词微波辐射酰化酯化反应硅胶固载催化剂
Abstract
Abstract

This thesis consist of three parts:
In the first part, the paper summarized microwave irradiation technology
increasing extensive application anic reactions in recent years. The advantage of
the microwave irradiation including rate enhancement, easy work up and high yield
has also been described in this paper.
In the second part, formic acid has been found to be an excellent formylating
agent to synthesize N-aryl formamides under microwave irradiation in good yields.
Compared with the traditional method, the reaction times are shortened 20-120 times.
The melt point of pound is consistent with the literature; the structure of
compound is also analyzed by IR.
In the third part, arylthiols react with chloropropionic acid to give
â-arylthiopropionic acid in good yield under microwave irradiation within short time
(3~4min). The â-arylthiopropionic acids obtained in the above procedure are cyclized
to give thiochroman-4-ones in the presence of polyphosphoric acid under microwave
irradiation. Compared with the classical methods the reaction time is shortened
hundreds times, operation is simple and the yield is high.
In the fourth part, Aryloxyacetate and arylthioacetate are wildly used in many
fields. Various methods have been developed for their synthesis. Some methods have
not been entirely satisfactory due to drawbacks such as long reaction time, emerging