亚铵阳离子型脱水剂制备与应用及氯化亚砜脱酰基保护

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1、密级：学校代码：10075分类号：学号：20091169理学硕士学位论文亚铵阳离子型脱水剂制备与应用及氯化亚砜脱酰基保护学位申请人：杜丁香指导教师：曹玉庆副教授学位类别：理学硕士学科专业：药物化学授予单位：河北大学答辩日期：二〇一二年六月ClassifiedIndex:CODE:10075U.D.C.:NO:20091169ADissertationfortheDegreeofM.SciencePreparationandApplicationofImmoniumTypeDehydratingAgentsandDeprotectionofAcylGroupforAmideswithT

2、hionylChlorideCandidate:DuDing-xiangSupervisor:ViceProf.CaoYu-QingAcademicDegreeAppliedfor:MasterofScienceSpecialty:PharmaceuticalChemistryUniversity:HebeiUniversityDateofOralExamination: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

3、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IAbstractAbstra

4、ctThisDissertationincludestwoparts,ontheonehand,anewpreparationmethodofImmoniumTypedehydratingagents:N,N-Dimethyl-N-phenoxymethyleneiminiumChloride(DMPhOMIC)isstudiedandthepreliminaryapplicationintheconversionofamidesintonitrileswerereported.Itwasanewandconvenientmethod,forithastheadvantagesofs

5、impleoperationandinexpensive.Ontheotherhand,deprotectionofaminogroupwiththionychloridewerecarriedout,whichhasthefeaturesofshortreactiontime,lowcostandeasypurification.Satisfactoryyieldswereobtained.Thisthesisconsistsofthreechapters:Chapter1:PrefaceChapter2:StudyonthepreparationofImmoniumTypedeh

6、ydratingagents:N,N-Dime-thyl-N-phenoxymethyleneiminiumChloride(DMPhOMIC)andAmideswereconvertedintocorrespondingnitrilesbyusingDMPhOMICasdehydratingagent.Theresultsshowedthatthemethodhasfeaturesoflowercost,easypurification,higheryieldandeaseofwork-up.Chapter3:Anewmethodisreported:Theprotectiongr

7、oupforaminoofamideswasremovedbythionylchlorideviachlorationandhydrolysiswithdichloromethaneassolventandtriethanolamineascatalyst.Themethodhasthefeatureofinexpensive,simpleoperation,shortreactiontime,easypurificationandmild.Keyword