| 5,6-二氢-4H-6-甲基噻嗯并[2,3-b]噻喃-4-酮-2-磺酰胺的合成 |
| |
| 引用本文： | 吴春姗,张珩,杨艺虹,杨建设,汪淼.5,6-二氢-4H-6-甲基噻嗯并[2,3-b]噻喃-4-酮-2-磺酰胺的合成[J].精细化工中间体,2007,37(3):38-40. |
| |
| 作者姓名： | 吴春姗 张珩 杨艺虹 杨建设 汪淼 |
| |
| 作者单位： | 武汉工程大学,湖北省新型反应器与绿色化学工艺重点实验室,湖北,武汉,430073 |
| |
| 摘 要： | 以丁烯酸和2-巯基噻吩为原料,经加成缩合制得3-(2-噻吩硫基)丁酸(2);以氯化亚砜氯化,三氯化铝催化环合得5,6-二氢-4H-6-甲基噻嗯并2,3-b]噻喃-4-酮(3);再经磺化、氯化、氨解反应合成得5,6-二氢-4H-6-甲基噻嗯并2,3-b]噻喃-4-酮-2-磺酰胺(1)。其中经均匀设计优化了环合反应条件为:n(2)∶n(氯化亚矾)∶n(三氯化铝)=1∶3∶1.5,于20℃反应2h。以2-巯基噻吩计,1合成总收率为30.49%,结构经IR、MS、1HNMR确证。
|
| 关 键 词： | 噻嗯并呋喃酮 盐酸杜噻酰胺 环合 |
| 文章编号： | 1009-9212（2007）03-0038-03 |
| 修稿时间： | 2007-01-26 |
Synthesis of 5,6-Dihydro-6- methyl-4H- thieno [2,3-b] thiopyrane-4-one-2-sulfonamide |
| |
| WU Chun-shan,ZHANG Heng,YANG Yi-hong,YANG Jian-she,WANG Miao.Synthesis of 5,6-Dihydro-6- methyl-4H- thieno [2,3-b] thiopyrane-4-one-2-sulfonamide[J].Fine Chemical Intermediates,2007,37(3):38-40. |
| |
| Authors: | WU Chun-shan ZHANG Heng YANG Yi-hong YANG Jian-she WANG Miao |
| |
| Abstract: | 3-(2-Mercaptothiophene)butanoic acid (2) was produced from crotonic acid and 2-mercaptothiophene,through condensation. 5,6-dihydro-6- methyl-4H- thieno2,3-b] thiopyrane-4-one(3)was produced through chlorination by thionyl chloride and cyclization by anhydrous of aluminium chloride,and then 5,6-dihydro-6- methyl-4H- thieno2,3-b]thiopyrane-4-one-2-sulfonamide(1)was produced through sulfonatio,chlorination and ammonolysis. The optimum technological condition gained through homogeneous design were as follow:n(2) ∶ n(SOCl2) ∶ n(AlCl3)=1 ∶ 3 ∶ 1.5,and reaction temperature was 20℃ for 2 hours. The total yield was 30.49% based on 2-mercaptothiophene. The products were characterized by IR ,MS and 1H NMR. |
| |
| Keywords: | thienothiopyrane dorzolamide hydrochloride cyclization |
| 本文献已被 CNKI 维普 万方数据 等数据库收录！ |
|
