文档介绍：大连理工大学硕士学位论文 3-(β-羟乙基砜基)-N-乙基苯胺的合成及反应机理的研究姓名:林乐森申请学位级别:硕士专业:精细化工指导教师:吴祖望 19990601 摘要本论文研究了3.(B一羟乙基砜基)一硝基苯在水介质中用Raney Ni作催化剂的加氢还原工艺咀及3一(B羟乙基砜基)一苯胺在Raney Ni催化下分别用乙醇和乙醛作烷化剂通过催化还原烷基化合成3一(B一羟乙基砜基)-N一乙基苯胺的工艺及其副反应。。 L3.()一硝基苯在水介质中用Raney Ni作催化剂的加氢还原,原料硝基物的转化率>99%,产品纯度>99%,%。 3一(B掘乙基砜基)一苯胺用乙醇作烷化剂,以重量为3一() 一苯胺40%的RaneyNi为催化剂,进行还原烷基化,产品纯压》85%,收爷850/o。其主要副反应是由于大量催化剂导致的C—S键的氢解反应。卜/7 用乙醛作烷化剂,催化剂RaneyNi用量可以降至原料3.(). 苯胺重量的10%,单烷化产品纯度95%以上,转怿98%。主要的副产物为3一()-N一乙基-N-(Ct-羟乙基)-苯胺和3,3 7一二(B一羟乙基砜基)-N,N 。且盎剧产物均可随着催化剂用量的增多及反应时间的延长氢解生成目标产物3.()-。 ABSTRAC丁·II· ABSTRACT An investigation ofthepreparation 3-(13-hydroxy-ethyl-sulfonyl)一 N—ethyl anilineby reductive alkylation LiIlLesen 3一(13一hydroxy-ethyl—sulfonyl)-N—ethyl anilineis ailimportant intermediate forbifuctional ethylgroupintroduced on thebridge nilrogen atom of theMCTNS bifimctionaldyeposseseshigherreactivity,goodpeⅡneabin妙and build-uppmpertieS and better fastness tochlorinebleach thanthatofimino bridge(no ethylldyes. Thetechniqueofhydrogenation of3--(13-hydroxy-ethyl-·sulfonyl)-nitrobenzene byRaney nickel catalysis inaqueous medium has been 99%conversion ofni∞ compound with>99%purity of3-(13-hydroxy-ethyl—sulfonyl)-aniline hasbeen achieved If the reaemnt 3-Ca-hydroxy-ethyl-sulfonyl)-nitrobenzene produced by ethylene oxide method,the presellce of alittleamount of artanionsurfactunt inthehydrogenation is required,which provide the reactant system good dispersivity ofthe reactant inaqueous mediun%SO assatisfactoryyeildofhydrogenation would be obtained Reduetivealkylafion of3-([3-hydroxy-ethyl·suifonyl)一aniline withethyl alcoholinthe presenceofRaney nickel as acatalyst,more than85%selectivity monoalkylation and95% conversion wereacheived,but theamount ofcatalyst usedinthereactionis≥40%ofthe mnottnt ofprimary tmsbeendetermined thatthe main by-products are - diethylaniline andN— woNd deduce thatthet