广东化工
廣東化工
엄동화공
GUANGDONG CHEMICAL INDUSTRY
2012年
14期
11-12
,共2页
王晓川%彭定芬%康富春%林东恩
王曉川%彭定芬%康富春%林東恩
왕효천%팽정분%강부춘%림동은
咪唑%固化剂%雷尼镍%脱氢%水解法
咪唑%固化劑%雷尼鎳%脫氫%水解法
미서%고화제%뢰니얼%탈경%수해법
imidazole%curing agent%Raney-Ni%dehydration%hydrolysis
以二乙烯三胺和乙酸为原料,通过成环、催化脱氢和水解三步反应合成了1-氨乙基-2-甲基咪唑。通过红外光谱、核磁共振氢谱和质谱对合成物进行了表征。结果表明:在n(二乙烯三胺)∶n(乙酸)=1∶2,升温至200℃关环脱水的条件下,生成N-(2-甲基-2-咪唑啉)乙基乙酰胺,达到92.3%的产率。然后,将该咪唑啉用雷尼镍催化脱氢生成对应的咪唑,产率94.0%。最后,将N-(2-甲基-2-咪唑)乙基乙酰胺用盐酸回流水解,得到的1-氨乙基-2-甲基咪唑,产率84.8%。
以二乙烯三胺和乙痠為原料,通過成環、催化脫氫和水解三步反應閤成瞭1-氨乙基-2-甲基咪唑。通過紅外光譜、覈磁共振氫譜和質譜對閤成物進行瞭錶徵。結果錶明:在n(二乙烯三胺)∶n(乙痠)=1∶2,升溫至200℃關環脫水的條件下,生成N-(2-甲基-2-咪唑啉)乙基乙酰胺,達到92.3%的產率。然後,將該咪唑啉用雷尼鎳催化脫氫生成對應的咪唑,產率94.0%。最後,將N-(2-甲基-2-咪唑)乙基乙酰胺用鹽痠迴流水解,得到的1-氨乙基-2-甲基咪唑,產率84.8%。
이이을희삼알화을산위원료,통과성배、최화탈경화수해삼보반응합성료1-안을기-2-갑기미서。통과홍외광보、핵자공진경보화질보대합성물진행료표정。결과표명:재n(이을희삼알)∶n(을산)=1∶2,승온지200℃관배탈수적조건하,생성N-(2-갑기-2-미서람)을기을선알,체도92.3%적산솔。연후,장해미서람용뢰니얼최화탈경생성대응적미서,산솔94.0%。최후,장N-(2-갑기-2-미서)을기을선알용염산회류수해,득도적1-안을기-2-갑기미서,산솔84.8%。
1-Aminoethyl-2-methylimidazole was synthesized from diethylenetriamine and acetic acid by cyclization,catalytic dehydration and hydrolysis reaction.The chemical struction was characterized by FT-IR,1H-NMR and MS.The experiment showed that when n(diethylenetriamine)∶n(acetic acid)=1∶2,elevating temperature to 200 ℃,the product was N-(2-methyl-2-imidazolinyl)ethyl acetamide with the yield of 92.3 %.The next reaction was dehydration of imidazoline to imidazole with Raney-Ni.The yield of this reaction was 94.0 %.Finally,1-Aminoethyl-2-methylimidazole could be got by hydrolysis reaction of N-(2-methyl-2-imidazolyl)ethyl acetamide with HCL and the yield was 84.8 %.