二茂铁硫代乙酰吗啉合成工艺的研究

Synthesis of Ferrocenyl Thioacetyl Morpholine

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-克酰基化反应合成单乙酰基二茂铁，并通过正交试验得出最佳条件：n（二茂铁）：n（乙酰氯）：n（氧化锌）=1:3:1.2时，产率为86%；然后将乙酰基二茂铁与单质硫、吗啉发生Willgerodt-Kinder反应，合成二茂铁硫代乙酰吗啉，通过正交试验得出最佳条件：n（乙酰基二茂铁）：n（单质硫）：n(吗啉)=1:3:6，反应温度128℃，反应时间4h，产率为65%，并经元素分析，IR，1HNMR表征确定为目标产物。

Abstract:

Acetylferrocene was synthesized via Friedel-Crafts acylation with ferrocene and acetyl chloride as raw material, dichloromethane as solvent, zinc oxide as catalyst. And optimal condition was concluded by orthogonal, its yield was 86% under the reaction conditions of molar ratio of ferrocene to acetyl chloride and zinc oxide 1:3:1.2. Ferrocenyl thioacetyl morpholine was synthesized via Willgerodt-Kinder reaction with acetylferrocene, sulfur and morpholine as starting material. The optimal condition was concluded by orthogonal, its yield was 65% under the reaction conditions of molar ratio of acetylferrocene to sulfur and Morpholine 1:3:6, reaction temperature was 128℃, reaction time was 4 hours.The product was characterized by elemental analysis, IR, 1HNMR.