化学通报(印刷版)
化學通報(印刷版)
화학통보(인쇄판)
CHEMISTRY
2010年
1期
83-87
,共5页
赵莹%赵芳%谭晓燕%李姣娟
趙瑩%趙芳%譚曉燕%李姣娟
조형%조방%담효연%리교연
AlCl_3%氰乙基化反应%取代苯胺%气相色谱分析
AlCl_3%氰乙基化反應%取代苯胺%氣相色譜分析
AlCl_3%청을기화반응%취대분알%기상색보분석
AlCl_3%Cyanoethylation%Substituted aniline%Gas chromatograph analysis
对于邻位、间位取代苯胺与丙烯腈发生单氰乙基反应生成相应的N-氰乙基邻位取代苯胺和N-氰乙基间位取代苯胺的过程,AlCl_3具有高的催化活性.在芳香胺/丙烯腈/AlCl_3=1/1.10/(0.05~0.10)(摩尔比)、反应温度60~80℃,反应时间6~10 h的条件下,反应的收率达87%~90%.用毛细管气相色谱法分析了单氰乙基化反应中各组份的含量;所合成的7种N-氰乙基邻位取代苯胺和N-氰乙基间位取代苯胺用DTA-TG、UV、IR、~1H NMR和EA进行了物性和结构表征.
對于鄰位、間位取代苯胺與丙烯腈髮生單氰乙基反應生成相應的N-氰乙基鄰位取代苯胺和N-氰乙基間位取代苯胺的過程,AlCl_3具有高的催化活性.在芳香胺/丙烯腈/AlCl_3=1/1.10/(0.05~0.10)(摩爾比)、反應溫度60~80℃,反應時間6~10 h的條件下,反應的收率達87%~90%.用毛細管氣相色譜法分析瞭單氰乙基化反應中各組份的含量;所閤成的7種N-氰乙基鄰位取代苯胺和N-氰乙基間位取代苯胺用DTA-TG、UV、IR、~1H NMR和EA進行瞭物性和結構錶徵.
대우린위、간위취대분알여병희정발생단청을기반응생성상응적N-청을기린위취대분알화N-청을기간위취대분알적과정,AlCl_3구유고적최화활성.재방향알/병희정/AlCl_3=1/1.10/(0.05~0.10)(마이비)、반응온도60~80℃,반응시간6~10 h적조건하,반응적수솔체87%~90%.용모세관기상색보법분석료단청을기화반응중각조빈적함량;소합성적7충N-청을기린위취대분알화N-청을기간위취대분알용DTA-TG、UV、IR、~1H NMR화EA진행료물성화결구표정.
Mono-cyanoethylation addition reactions of o-substituted or m-substituted anilines with acrylonitrile have been carried out in the presence of AlCl_3 , resulting in N-β-cyanoethyl-α-substituted anilines, N-β-cyanoethyl-m-substituted anilines in high yield. Under the conditions of mole ratio of the reactants as substituted anilines: acrylonitrile: AlCl_3 = 1 : 1.10: (0. 05~0. 10), the temperature of 60~80℃ for 6~10 h, the yields of mono-cyanoethyl substituted anilines were 87 %~90 % , and capillary gas chromatographic determination method was used for the contents analysis of N-β-cyanoethyl-o-substituted anilines or N-β-cyanoethyl-p-substituted anilines amongmono-cyanoethylation reactions. All of products were characterized by DTA-TG, UV-Vis, FTIR,~1H NMR, andelemental analyses.