亚铵阳离子型脱水剂制备与应用及氯化亚砜脱酰基保护.pdf

Classified Index: CODE: 10075 U.D.C.: NO: A Dissertation for the Degree of M. Science Preparation and Application of Immonium Type Dehydrating Agents and Deprotection of Acyl Group for Amides with Thionyl Chloride Candidate: Du Ding-xiang Supervisor: Vice Prof. Cao Yu-Qing Academic Degree Applied for: Master of Science Specialty: Pharmaceutical Chemistry University: Hebei University Date of Oral Examination: June，2012 摘 要 摘 要 本文主要研究了两部分内容，一部分是亚铵阳离子型脱水剂苯氧甲烯基二甲基氯化 铵（DMPhOMIC ）的制备及其应用于酰胺制备腈的反应,该方法操作简单，原料价格便 宜，产率高。另外一部分是氯化亚砜脱氨基的乙酰基保护反应，此法试剂廉价易得，反 应时间短，易分离纯化。两部分均获得了较理想的结果。全文共分为三章。 第一章：前言。 第二章：研究了亚铵阳离子型脱水剂DMPhOMIC 的制备及酰胺类化合物在脱水剂 DMPhOMIC 的作用下得到相应的腈类化合物。该法具有反应速率快，操作方便，原料 价格便宜,成本低，后处理简单，产率较高等特点。 第三章：介绍了一种以二氯甲烷为溶剂，三乙胺为催化剂，氯化亚砜与酰胺类化合 物经氯化、水解两步脱除氨基乙酰基保护的新方法，此法所用试剂价廉易得，反应时间 短，条件温和，操作方便，后处理简单等特点。 关键词 亚胺阳离子型脱水剂 酰胺 腈 氯化亚砜 脱酰基保护 I Abstract Abstract This Dissertation includes two parts,on the one hand,a new preparation method of Immonium Type dehydrating agents :N,N -Dimethyl-N -phenoxymethyleneiminium Chloride (DMPhOMIC) is studied and the preliminary application in the conversion of amide s into nitriles were reported.It was a new and convenient method,for it has the advantages of simple operation and inexpensive.On the other hand,deprotection of amino group with thiony chloride were carried