| 微波辐射合成5-氨基-噻唑[4,5-d]嘧啶-2(3H)-酮 |
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| 引用本文： | 薛峰,渠桂荣,韩素辉.微波辐射合成5-氨基-噻唑[4,5-d]嘧啶-2(3H)-酮[J].精细化工,2006,23(4):407-410. |
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| 作者姓名： | 薛峰 渠桂荣 韩素辉 |
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| 作者单位： | 河南师范大学,化学与环境科学学院,河南,新乡,453007;河南师范大学,化学与环境科学学院,河南,新乡,453007;河南师范大学,化学与环境科学学院,河南,新乡,453007 |
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| 摘 要： | 以硫脲和氯乙酸为原料,在无溶剂和350 W微波辐射4 m in条件下,缩合生成中间体2,4-噻唑烷二酮(Ⅰ)产率91.5%;随后在无溶剂和400 W微波辐射5 m in条件下,通过V ilsm e ier甲酰化反应,生成中间体4-氯-5-甲酰基噻唑-2(3H)-酮(Ⅱ),产率86.7%;最后以正丙醇为溶剂,450 W微波辐射7 m in条件下,成环得到5-氨基-噻唑4,5-d]嘧啶-2(3H)-酮(Ⅲ),产率80.5%。反应总产率为63.9%。合成产物与中间体的结构经1HNMR,MS和元素分析确认。
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| 关 键 词： | 5-氨基-噻唑[4 5-d]嘧啶-2(3H)-酮 4-氯-5-甲酰基噻唑-2(3H)-酮 微波辐射 |
| 文章编号： | 1003-5214(2006)04-0407-04 |
| 收稿时间： | 2005-07-14 |
| 修稿时间： | 2005-07-142005-11-03 |
Synthesis of 5-Amino-thiazolo[4,5-d]pyrimidin-2(3H)-one Under Microwave Irradiation |
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| XUE Feng,QU Gui-rong,HAN Su-hui.Synthesis of 5-Amino-thiazolo[4,5-d]pyrimidin-2(3H)-one Under Microwave Irradiation[J].Fine Chemicals,2006,23(4):407-410. |
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| Authors: | XUE Feng QU Gui-rong HAN Su-hui |
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| Affiliation: | College of Chemistry and Environmental Science, Henan Normal University, Xinxiang 453007, Henan, China |
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| Abstract: | Condensation of thiourea and chloroacetic acid under solvent-free microwave irradiation of 350 W and 4 min gave 2,4-thiazolidinedione(Ⅰ) in 91.5%yield.Then,4-chloro-5-formylthiazol-2(3H)-one(Ⅱ) was obtained in 86.7% by Vilsmeier reaction of Ⅰ under solvent-free microwave irradiation of 400 W and 5 min.Finally,under microwave irradiation of 450 W and 7 min,5-amino-thiazolopyrimidin-2(3H)-one(Ⅲ)was synthesized in 80.5% yield fromⅡ and guanidine hydrochloride with n-propanal as solvent through cyclization reaction.The total yield of Ⅲ was 63.9%.Final product as well as the intermediate was identified by ~1HNMR,MS and elementary analysis. |
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| Keywords: | 5-amino-thiazolopyrimidin-2(3H)-one 4-chloro-5-formylthiazol-2(3H)-one microwave irradiation |
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