| 6-氨基-4-苯基-2-碳硫双键-1,2-二氢嘧啶-5-甲酰胺的合成条件优化 |
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| 引用本文： | 马世堂,方百欢,仝清晨,王金萍,时 新.6-氨基-4-苯基-2-碳硫双键-1,2-二氢嘧啶-5-甲酰胺的合成条件优化[J].贵州师范大学学报(自然科学版),2014(2):104-106. |
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| 作者姓名： | 马世堂 方百欢 仝清晨 王金萍 时 新 |
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| 作者单位： | 安徽科技学院食品药品学院,安徽凤阳233100 |
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| 基金项目： | 安徽省教育厅高校省级自然科学项目（kj2013z055）;安徽科技学院青年基金（ZRC2013341）;国家重大新药创制（2012ZX09303009_002） |
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| 摘 要： | 以氰基乙酰胺、硫脲、苯甲醛为原料,一锅煮法合成6-氨基-4-苯基-2-碳硫双键-1,2-二氢嘧啶-5-甲酰胺,并对反应温度、反应时间、原料的投料比、反应介质以及对收率影响进行考察,产物经核磁进行表征。结果:在催化剂四水乙酸镍催化下,以氰基乙酰胺、硫脲、苯甲醛为原料发生"一锅煮"的3组分反应得到目标物,在氮气保护下并确定反应温度在70℃下回流反应7h,以1.0∶1.2∶1.5mmol投料比在THF中进行反应。本方法简单、产率高,节约时间和环境友好。
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| 关 键 词： | 6-氨基-4-苯基-2-碳硫双键-1 2-二氢嘧啶-5-甲酰胺 TLC跟踪 一锅法合成 氢谱 |
Synthesis of 6-amino-4-phenyl-2-sulfanylidene-1,2-dihydropyrimidine-5-carboxamide compounds |
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| MA Shitang,FANG Baihuan,TONG Qingchen,WANG Jinping,SHI Xin.Synthesis of 6-amino-4-phenyl-2-sulfanylidene-1,2-dihydropyrimidine-5-carboxamide compounds[J].Journal of Guizhou Normal University(Natural Sciences),2014(2):104-106. |
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| Authors: | MA Shitang FANG Baihuan TONG Qingchen WANG Jinping SHI Xin |
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| Institution: | (Food and Drug College, Anhui Science and Technology University, Fengyang, Anhui 233100, China) |
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| Abstract: | The process of preparing 6-amino-4-phenyl-2-sulfanylidene-1,2-dihydropyrimi-dine-5-carboxamide was investigated.Synthesis via one-pot reaction of cyanoacetamide、thiourea 、benzaldehyde using tetrahydrated nickel acetate as catalyst.The effect of reaction conditions on the yield was then inquired.The optimal reaction process were as follows：reaction with a nitrogen inletat 70 ℃ for 7 h,the raw ratio was 1.0：1.2：1.5,tetrahydrated nickel acetate as catalyst.this is a simple 、highly-yielding、time-saving and environmentally friendly method. |
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| Keywords: | 6-amino-4-phenyl-2-sulfanylidene-1 2-dihydropyrimidine-5-carboxamide TLC tracking one-pot synthesis 1H-NMR |
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