| 第 36 卷第 5 期 |  | Vol. 36 No. 5 | | 2006 年 10 月 | Oct 2006 |
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所屬欄目：醫藥及中間體
阿巴卡韋中間體2-雜氮雙環(huán)[2,2,1]庚-5-烯-3-酮的合成 |
| 陳燦; 郭莉娜; 李宏偉; 侯仲軻(湖南化工研究院藥物研究所; 華中師范大學(xué); 湖南長(cháng)沙; 湖北武漢) |
| 摘 要：采用一步法由對甲基苯亞磺酸鈉與氯化氰及1,3-環(huán)戊二烯合成目標物2-雜氮雙環(huán)[2,2,1]庚-5-烯-3-酮。反應條件為:n(對甲基苯亞磺酸鈉)∶n(氯化氰)∶n(1,3-環(huán)戊二烯)=0.48∶1.05∶1,反應溫度控制在15℃,反應7h,反應中控制pH=5,可得純度為95%的產(chǎn)品,收率由文獻報道的64%提高到78%。 |
| 關(guān)鍵詞：一步法; 合成; 2-雜氮雙環(huán)[2; 2; 1]庚-5-烯-3-酮 |
| 中圖分類(lèi)號：TQ463 文獻標識碼：A 文章編號：1009-9212(2006)05-0036-03 |
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| Synthesis of 2-Azabicyclohept-5-en-3-one as an Intermediate for Abacavir |
| CHEN Can1; GUO Li-na2; LI Hong-wei2; HOU Zhong-ke1（1.Institute of Pharmaceuticals; Hunan Research Institute of Chemical Industry; Changsha 410007; China; 2.Central China Normal University; Wuhan 430079; China） |
| Abstract：2-Azabicyclohept-5-en-3-one was synthesized from sodium-p-toluene sulfinate with cyanogens chloride and cyclopentadiene by one-pot process.The optimal conditions were as follow: the mole ratio of sodium-p-toluene sulfinate:cyanogens chloride:cyclopentadiene was 0.48∶1.05∶1,the reaction temperature 15℃,reaction time 5 h and pH of the reaction 5.Under these optimal conditions,the purity of product was 95%,and The yield was increased from 64% to 78%. |
| Key words：one-pot process; synthesis; 2-azabicyclohept-5-en-3-one |
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收稿日期：2006-07-12
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