二茂铁硫代乙酰吗啉合成工艺  

Synthesis of Ferrocenyl Thioacetyl Morpholine

作　　者：刘玉婷[1,2] 陈丹[1,2] 尹大伟[1,2] 

机构地区：[1]陕西科技大学教育部轻化工助剂化学与技术重点实验室,陕西西安710021 [2]陕西科技大学化学与化工学院,陕西西安710021

出　　处：《精细化工》2010年第9期879-881,907,共4页Fine Chemicals

基　　金：陕西省自然科学基础研究计划重点项目(2009JZ002);陕西科技大学博士基金资助项目(05BJ-1)~~

摘　　要：以二茂铁和乙酰氯为原料,二氯甲烷为溶剂,氧化锌为催化剂,进行傅-克酰基化反应合成乙酰基二茂铁(主产物为单乙酰基二茂铁),并通过正交实验得出最佳反应条件:n(二茂铁)∶n(乙酰氯)∶n(氧化锌)=1∶3∶1.2,反应时间45 min,在该条件下产率为86%;然后,乙酰基二茂铁与硫磺、吗啉发生Willgerodt-Kinder反应,合成二茂铁硫代乙酰吗啉,通过正交实验得出最佳条件:n(乙酰基二茂铁)∶n(硫磺)∶n(吗啉)=1∶3∶6,反应时间4 h,在该条件下产率为65%,并经元素分析、IR、1HNMR表征确定为目标产物。Acetylferrocene（main product is monoacetylferrocene） was synthesized via the Friedel-Crafts acylation with ferrocene and acetyl chloride as raw materials,dichloromethane as solvent,zinc oxide as catalyst.The optimal condition was concluded by the orthogonal experiment.Its yield was 86% under the reaction conditions of the molar ratio of ferrocene to acetyl chloride and zinc oxide 1∶3∶1.2,reaction time 45 min.Ferrocenyl thioacetyl morpholine was synthesized via the Willgerodt-Kinder reaction with acetylferrocene,sulfur and morpholine as starting materials.The optimal condition was concluded by the orthogonal experiment.Its yield was 65% under the reaction conditions of the molar ratio of acetylferrocene to sulfur and morpholine 1∶3∶6,reaction time was 4 hours.The product was characterized by elementary analysis,IR,1HNMR.

关 键 词：二茂铁 傅-克酰基化 Willgerodt—Kinder反应 二茂铁硫代乙酰吗啉 医药原料 

分 类 号：O622.7[理学—有机化学]