应用化学
應用化學
응용화학
CHINESE JOURNAL OF APPLIED CHEMISTRY
2009年
10期
1206-1210
,共5页
三氯化铁%Biginelli缩合反应%二氢嘧啶%一锅合成%微波辐射
三氯化鐵%Biginelli縮閤反應%二氫嘧啶%一鍋閤成%微波輻射
삼록화철%Biginelli축합반응%이경밀정%일과합성%미파복사
ferric chloride%Biginelli condensation%dihydropyrimidine%one-pot synthesis%microwave irradiation
以FeCl_3·6H_2O为催化剂,无水乙醇为溶剂,n(取代-4-甲酰基吡唑):n(乙酰乙酸乙酯):n((硫)脲):n(FeCl_3)·n(6H_2O)=1:3:3:1,采取微波辐射和常规加热回流的方法,通过Biginelli缩合反应一锅合成了6种新型含吡唑基的3,4-二氢嘧啶类化合物,并进行了元素分析、IR、~1H NMR和~(13)C NMR表征,对反应机理和化合物的图谱特征进行了探讨. 结果表明,利用微波辐射法合成含吡唑基3,4-二氢嘧啶类化合物具有反应时间短,产率高等优点.
以FeCl_3·6H_2O為催化劑,無水乙醇為溶劑,n(取代-4-甲酰基吡唑):n(乙酰乙痠乙酯):n((硫)脲):n(FeCl_3)·n(6H_2O)=1:3:3:1,採取微波輻射和常規加熱迴流的方法,通過Biginelli縮閤反應一鍋閤成瞭6種新型含吡唑基的3,4-二氫嘧啶類化閤物,併進行瞭元素分析、IR、~1H NMR和~(13)C NMR錶徵,對反應機理和化閤物的圖譜特徵進行瞭探討. 結果錶明,利用微波輻射法閤成含吡唑基3,4-二氫嘧啶類化閤物具有反應時間短,產率高等優點.
이FeCl_3·6H_2O위최화제,무수을순위용제,n(취대-4-갑선기필서):n(을선을산을지):n((류)뇨):n(FeCl_3)·n(6H_2O)=1:3:3:1,채취미파복사화상규가열회류적방법,통과Biginelli축합반응일과합성료6충신형함필서기적3,4-이경밀정류화합물,병진행료원소분석、IR、~1H NMR화~(13)C NMR표정,대반응궤리화화합물적도보특정진행료탐토. 결과표명,이용미파복사법합성함필서기3,4-이경밀정류화합물구유반응시간단,산솔고등우점.
Pyrazol-3,4-dihydropyrimidines were synthesized by one-pot Biginelli cyclocondensation of substituted-4-formylpyrazole， ethyl acetoacetate， urea or thiourea and ferric choride(in molar ratio of 1∶ 3∶ 3∶ 1) in ethanol, under traditional heating or microwave irradiation conditions, while ferric chloride was used as a catalyst. The structures of all the products were characterized by elemental analysis, IR, ~1H NMR and ~(13)C NMR. The mechanism of the reaction and the spectra of all the compounds were also discussed. The method of microwave irradiation showed some advantages, such as a shorter reaction time and a higher yield, which is a new approach for synthesizing this kind of compounds.
