海南师范大学学报(自然科学版)
海南師範大學學報(自然科學版)
해남사범대학학보(자연과학판)
JOURNAL OF HAINAN NORMAL UNIVERSITY(NATURAL SCIENCE)
2015年
1期
47-48,58
,共3页
刘冲%李国柱%凤翠%丛榕%刘风娇%方俊逸%江杰%吴明书
劉遲%李國柱%鳳翠%叢榕%劉風嬌%方俊逸%江傑%吳明書
류충%리국주%봉취%총용%류풍교%방준일%강걸%오명서
5-甲氧基靛红%Sandmeyer 合成法%靛红衍生物
5-甲氧基靛紅%Sandmeyer 閤成法%靛紅衍生物
5-갑양기전홍%Sandmeyer 합성법%전홍연생물
5-methoxy-isatin%Sandmeyer method%Isatin derivatives
从5-甲氧基苯胺出发,探索出了用Sandmeyer法两步合成目标分子5-甲氧基靛红的合成方法,找到了合成目标分子的最佳条件:以水为溶剂,在90℃条件下,5-甲氧基苯胺与水合氯醛,盐酸羟胺反应3.5 h,得到对甲氧基异亚硝基乙酰苯胺,产率95%.在92℃,浓H2SO4(75%)条件下环合,经水解后得到5-甲氧基靛红,产率为88%.使用该方法合成5-甲氧基靛红,反应操作简便高效.
從5-甲氧基苯胺齣髮,探索齣瞭用Sandmeyer法兩步閤成目標分子5-甲氧基靛紅的閤成方法,找到瞭閤成目標分子的最佳條件:以水為溶劑,在90℃條件下,5-甲氧基苯胺與水閤氯醛,鹽痠羥胺反應3.5 h,得到對甲氧基異亞硝基乙酰苯胺,產率95%.在92℃,濃H2SO4(75%)條件下環閤,經水解後得到5-甲氧基靛紅,產率為88%.使用該方法閤成5-甲氧基靛紅,反應操作簡便高效.
종5-갑양기분알출발,탐색출료용Sandmeyer법량보합성목표분자5-갑양기전홍적합성방법,조도료합성목표분자적최가조건:이수위용제,재90℃조건하,5-갑양기분알여수합록철,염산간알반응3.5 h,득도대갑양기이아초기을선분알,산솔95%.재92℃,농H2SO4(75%)조건하배합,경수해후득도5-갑양기전홍,산솔위88%.사용해방법합성5-갑양기전홍,반응조작간편고효.
Two-step synthesis of 5-MeO isatin using 5-MeO aniline with the method called Sandmeyer has been ex?plored. The optimum reaction condition for the synthesis of 2-(hydroxyimino)-N-(4-methoxyphenyl)acetamide is in water, three components 5-MeO aniline and chloral hydrate and hydroxylamine hydrochloride as bases have been reacting together at 90℃for 3.5 hours,leading to the desired product in 95%yield. After acid hydrolysis with concentrated sulfuric acid(75%) at 92℃, 5-MeO isatin will be gained with 88%of yield. Therefore,with this highly efficient method, 5-MeO isatin can be prepared in a large scale in laboratory.