| 2,5-二取代1,3,4-噻二唑的合成 |
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| 引用本文： | 周艳芬,陈宏博. 2,5-二取代1,3,4-噻二唑的合成[J]. 辽东学院学报(自然科学版), 2009, 16(2) |
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| 作者姓名： | 周艳芬 陈宏博 |
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| 作者单位： | 大连理工大学精细化工国家重点实验室,辽宁,大连,116012 |
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| 摘 要： | 以5-氨基-2-巯基-1,3,4-噻二唑为原料,经过氨基酰基化、氯气氧化制得5-乙酰胺基-1,3,4-噻二唑-2-磺酰氯,该化合物与N-甲基哌嗪、苯胺反应,合成两个未见报道的目标产物:5-乙酰胺基-1,3,4-噻二唑-2-(N-甲基哌嗪磺酰胺)和5-乙酰胺基-1,3,4-噻二唑-2-(磺酰苯胺)。结果表明:原料酰基化的最佳条件为:物料的物质的量之比n(噻二唑)∶n(乙酸酐)=1∶1.25,反应温度为70℃,冰醋酸12 mL条件下,薄层色谱点板跟踪反应进程,目标产物収率为88%以上;目标化合物的最佳条件为:乙醇作溶剂,物料比1∶2,薄层色谱点板跟踪反应进程,室温条件下目标产物收率在88%以上,产品纯度均在97%以上。并利用IR1、H-NMR、LC-MS对目标产物进行表征。
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| 关 键 词： | 5-氨基-2-巯基-1,3,4-噻二唑 5-乙酰胺基-1,3,4-噻二唑-2-磺酰氯 N-甲基哌嗪 5-乙酰胺基-1,3,4-噻二唑-2-(N-甲基哌嗪磺酰胺) 5-乙酰胺基-1,3,4-噻二唑-2-(磺酰苯胺) |
Sythesis of 2,5-disubstitute-1,3,4-thiadiazole |
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| ZHOU Yan-fen,CHEN Hong-bo. Sythesis of 2,5-disubstitute-1,3,4-thiadiazole[J]. Journal of Liaodong University(Natural Sciences), 2009, 16(2) |
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| Authors: | ZHOU Yan-fen CHEN Hong-bo |
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| Affiliation: | ZHOU Yan-fen,CHEN Hong-bo(State Key Laboratory of Fine Chemicals,Dalian University of Technology,Dalian 116012,China) |
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| Abstract: | 5-acetylamino-1,3,4-thiadiazole-2-sulfonyl chloride compound was synthesized using 5-amino-2-mercapto-1,3,4-thiadiazole which was acidylated and oxidized with gaseous chlorine.By its reaction with N-methyl piperazine and aniline,two new target produces were obtained as 5-acetylamino-1,3,4-thiadiazole-(2-N-methyl piperazine) sulfonylanilin and 5-acetylamino-1,3,4-thiadiazole-(2-sulfonyl)-aniline.The results showed that the best acidylation conditions for raw materials were as follows: the proportion of 5-ami... |
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| Keywords: | 5-amino-2-mercapto-1 3 4-thiadiazole N-methyl piperazine 5-acetylamino-1 4thiadiazole-2-sulfonyl chloride 4-thiadiazole-(2-N-methyl piperazine) sulfonylanilin 4-thiadiazole-(2-sulfonyl)-aniline |
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