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机构地区:[1]中北大学化工与环境学院,山西太原030000
出 处:《化学试剂》2014年第5期475-477,480,共4页Chemical Reagents
摘 要:以盐酸羟胺、三乙胺和丁二酸酐为原料,以1,4-二氧六环和少量的水为溶剂,EDTA三钠盐为稳定剂,以1-羟基苯并三氮唑(HOBT)为催化剂,一步反应制得标题化合物。当n(盐酸羟胺)∶n(丁二酸酐)∶n(EDTA三钠盐)∶n(1-羟基苯并三氮唑)=1.01∶1∶0.000 3∶0.01,溶剂V(二氧六环)∶V(水)=20∶1,中和反应温度为20℃,后续反应温度为120℃,反应时间为6 h时,高真空除水,反应收率达87.5%,产品纯度≥99.6%。N-Hydroxysuccinimide was synthesized in a one- step process with hydroxylamine hydrochloride, triethylamine and succinie anhydride as the raw materials, 1,4-diethy]ene dioxide and water as the solvent, EDTA trisodium salt as the stabilizer, N-hydroxybenzotirzole as the catalyst. When the molar concentration ratio for hydroxylamine hydrochloride,succinic anhydride, EDTA trisodium salt and nhydroxy- benzotirzole is 1.01 : 1 : 0. 000 3 : 0. 01, the solvent ratio for 1,4-diethylene dioxide and water is 20:1 ,the neutral reac- tions temperature is 20 ℃, subsequent reactions temperature is 120 ℃ ,and the reaction time is 6 h, dehydrate at a high vacuum,yield up to 87.5% as well as the purity for product over 99. 6%.
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