二茂铁硫代乙酰吗啉合成工艺的研究

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。

Synthesis of Ferrocenyl Thioacetyl Morpholine

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.