摘要
采用一步法由对甲基苯亚磺酸钠与氯化氰及1,3-环戊二烯合成目标物2-杂氮双环[2,2,1]庚-5-烯-3-酮。反应条件为:n(对甲基苯亚磺酸钠)∶n(氯化氰)∶n(1,3-环戊二烯)=0.48∶1.05∶1,反应温度控制在15℃,反应7h,反应中控制pH=5,可得纯度为95%的产品,收率由文献报道的64%提高到78%。
2-Azabicyclo [2,2,1]hept-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%.
出处
《精细化工中间体》
CAS
2006年第5期36-38,共3页
Fine Chemical Intermediates