摘要
利用微波辅助技术，以3-氨基吡唑-4-甲酰胺、3-氨基吡唑-4-甲酸乙酯为原料合成新型毗唑化合物--3-甲酰氨基吡唑-4-甲酰胺、3-甲酰氨基吡唑4-甲酸乙酯，系统的研究了反应时间、反应温度、原料配比以及催化剂用量对反应的影响，确定该反应的最优化反应条件：3-氨基吡唑-4-羰基取代化合物与甲酰胺的比例1：4，催化剂用量为甲酰胺的1％-1．5％，100℃下反应40min，产品收率达90．5％，纯度〉97％。目标化合物结构经红外光谱、核磁共振等分析方法验证。
By means of the microwave assisted organic synthesis,new pyrazole derivatives,3-(formylamino)-1H-pyrazole-4-carboxamide and 3-(formylamino)-1H-pyrazole-4-carboxylate,were prepared from 3-amino-1H-pyrazole-4-carboxamide and 3-amino-1H-pyrazole-4-carboxylate.Main factors such as the reaction time,reaction temperature,raw materials ratio,and catalyst dosage were studied and the reaction mechanism was defined.The optimal reaction conditions were as follows:The reaction was conducted at 100 ℃ for 40 min at a ratio of 3-amino-1H-pyrazole-4-carboxamide(or 3-amino-1H-pyrazole-4-carboxylate)/formylamine equating to 1∶4 with a catalyst dosage of 1%～1.5%(based on the mass of formylamine),and the product yield was up to 90.5% with its purity reaching 97%.The product structure was confirmed by IR and NMR spectroscopy.
出处
《化学试剂》
CAS
CSCD
北大核心
2011年第2期164-166,共3页
Chemical Reagents
基金
国家高技术研究发展计划(863计划)重点项目(2008AA031202)
重庆市天然气化工重大科技专项资助项目(CSTC2008-AA4026)
中国博士后基金资助项目(20080430747)
