| 2-氨基-5-(4-甲氧苯基)-1,3,4-二唑的合成工艺研究 |
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| 引用本文： | 罗振华,吴疆,陈宝泉,曹东华.2-氨基-5-(4-甲氧苯基)-1,3,4-二唑的合成工艺研究[J].化学试剂,2012(6):549-551. |
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| 作者姓名： | 罗振华 吴疆 陈宝泉 曹东华 |
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| 作者单位： | 天津理工大学化学化工学院 |
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| 基金项目： | 国家自然科学基金资助项目(20971097);教育部大学生创新性实验计划项目(2010) |
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| 摘 要： | 以对甲氧基苯甲醛为原料,通过腙化、分子内环化两步反应合成了标题化合物。实验考察了投料物质的量比,反应温度及反应时间对收率的影响,结果表明:盐酸氨基脲与对甲氧基苯甲醛的物质的量比为1.2∶1,第1步反应温度为65℃,反应时间为1.5 h,第2步反应时间为16 h,溴与1-对甲氧基苯甲亚甲基氨基脲的物质的量比为1.2∶1时为最佳反应条件,总收率68.5%。目标化合物结构经红外光谱、核磁共振氢谱及质谱等确证。
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| 关 键 词： | 对甲氧基苯甲醛 盐酸氨基脲 2-氨基-5-(4-甲氧苯基)-1 3 4-二唑 合成 |
Synthesis of 2-amino-5-(4-methoxyphenyl)-1,3,4-oxadiazoles |
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| LUO Zhen-hua,WU Jiang,CHEN Bao-quan,CAO Dong-hua.Synthesis of 2-amino-5-(4-methoxyphenyl)-1,3,4-oxadiazoles[J].Chemical Reagents,2012(6):549-551. |
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| Authors: | LUO Zhen-hua WU Jiang CHEN Bao-quan CAO Dong-hua |
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| Affiliation: | (School of Chemistry and Chemical Engineering,Tianjin University of Technology,Tianjin 300384,China) |
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| Abstract: | 2-Amino-5-(4-methoxyphenyl)-1,3,4-oxadiazoles was synthesized from p-anisaldehyde by hydrazone reaction and intramolecular cyclization.The effects of time,temperature and reactants ratio on the yield were discussed.The results indicate that the molar ratio of p-anisaldehyde and semicarbazide hydrochloride is 1.2∶1,hydrazone reaction temperature 65 ℃,hydrazone reaction time 1.5 h,intramolecular cyclization time 16 h,n(Br2)∶n(4-methoxybenzaldehyde semicarbazone)=1.2∶1.The total yield was 68.5% and the structure of product was confirmed by IR,1HNMR and MS. |
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| Keywords: | p-anisaldehyde semicarbazide hydrochloride 2-amino-5-(4-methoxyphenyl)-1 3 4-oxadiazoles synthesis |
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