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机构地区:[1]宁夏大学化学化工学院,宁夏银川750021 [2]大连理工大学精细化工国家重点实验室,辽宁大连116024
出 处:《河北师范大学学报(自然科学版)》2015年第3期232-238,共7页Journal of Hebei Normal University:Natural Science
基 金:国家科技支撑计划(2011BAE07B01)
摘 要:以N,N-二甲基甲酰胺(DMF)为溶剂、三乙胺为缚酸剂,以对乙酰氨基苯磺酰氯、乙二胺为原料,经胺化、水解反应制备了活性染料中间体——N,N′-二(4-氨基苯基)磺酰乙二胺.用FTIR,MS,1 HNMR表征了该物质的结构,研究了其紫外吸收和荧光光谱性质,通过实验建立了关键步骤胺化反应的优化条件,n(对乙酰氨基苯磺酰氯)∶n(乙二胺)∶n(三乙胺)=2.1∶1.0∶2.4、投料温度0~10℃、胺化反应温度30℃、反应时间2h.结果表明,该物质的收率83.6%,纯度98.93%(HPLC).Using N, N-dimethyl formamide as orannic solvents and triethylamine as acid-binding agent, p-acetamidobenzene sulfonyl chloride and ethylenediamine as the raw materials,a reactive dye intermediates 4,4'-dianimo-N,N'-diphenylsulfonyl ethylenediamine was synthesized through two-step reactions of amina- tion and hydrolysis. The structure of product was characterized by means of FTIR, MS and ~HNMR. The UV spectra and the fluorescent spectrum were studied. The optimization conditions of amination,and the key step of synthesis,were set up through experiments:the molar ratio of n(p-acetamidobenzene sulfonyl chloride) : n(ethylenediamine) : n(triethylamine) was 2.1 : 1.0 : 2.4,feeding temperature was 0-10 ℃ , amination temperature was 30 ℃, reaction time was 2 h. The yield of product can reach 83.6%~ with the pu- rity of 98.93 %(HPLC).
关 键 词:N N′-二(4-氨基苯基)磺酰乙二胺 胺化条件 活性染料中间体
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