摘要
以1,5-二乙氧基-2,4-二硝基苯为原料,乙醇为溶剂,经铁粉还原得4,6-二乙氧基间苯二胺,较佳工艺条件为:V(水)∶V(乙醇)=1∶4.5,反应温度80℃,反应时间2h,滤液在氯化亚锡保护下加入盐酸后制得盐酸盐,旋蒸浓缩,-20℃下静置16h析出产物,氮气吹干,收率88%,纯度大于99%。又以4,6-二乙氧基间苯二胺为原料合成衍生物Ⅰ—Ⅴ,结构经FT-IR、13 C NMR和1 H NMR表征确认,并对其在大分子、染料以及材料方面的应用进行了分析.
Through reduction reaction,4,6-diethoxybenzene-1,3-diamine was synthesized from 1, 5-diethoxy-2,4-dinitrobenzene. Proper experimental conditions for the reduction reaction were found as.ethanol as solvent, V(water) : V(ethanol)= 1 : 4. 5, reaction temperature 80℃, reaction time 2 h, filtrate protected by stannous chloride and hydrochloric acid,precipitation under -20℃ within 16 h, dried by blowing with nitrogen, the yield of 4,6-diethoxybenzene-1,3-diamine hydrochloride was 88% based on 1,5-diethoxy-2,4-dinitrobenzene and the purity was more than 99% as determined by HPLC. And using 4, 6-diethoxybenzene-1,3-diamine as raw material, compounds I-V were synthesized. The structures of the compounds were characterized and conformed by FT-IR,^13C NMR and 1H NMR. And the applications in macromolecular, dye and material fields were discussed.
出处
《浙江工业大学学报》
CAS
2013年第6期624-629,共6页
Journal of Zhejiang University of Technology
基金
江苏省重大科技支撑计划项目(BE2011129)
关键词
4
6-二乙氧基间苯二胺
还原
衍生物
4,6-diethoxybenzene-1,3-diamine
applications
derivatives