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3-氯-1-(2-噻吩)-丙酮合成工艺的研究
Synthesis of 3-Chloro-1-(2-Thienyl)-Propone
【摘要】 3-氯-1-(2-噻吩)-丙酮是合成度洛西汀的中间体。通过对傅克酰基化反应制备该中间体工艺条件的研究,以CS2为溶剂,当噻吩、氯丙酰氯和无水氯化铝的摩尔比为1∶1∶1.5时,0℃反应2 h,可得到较好的收率。在后处理上,通入HCl加成来促使副产物向产物转化,大大提高了产物的收率,3-氯-1-(2-噻吩)-丙酮纯度96.86%,收率达87.51%。
【Abstract】 3-Chloro-1-(2-thienyl)-propone was prepared by friedel-crafts acylation of thiophene and 3-chloropropanyl chloride.Effects of catalyst,feedstock dosage,reaction temperature,reaction time,solvent and addition method on reaction were investigated.Under the preferably reaction conditions of 0 ℃,mole ratio of thiophene to 3-chloropropanyl chloride to aluminum chloride anhydrous 1∶1∶1.5 and CS2 as solvent,then the addition of anhydrous hydrochloric acid promoting conversion of byprodrct to major product,the finally purity and yield of 3-chloro-1-(2-thinly)-propone were 96.86% and 87.51% respectively.
【Key words】 friedel-crafts acylation; thiophene; 3-chloropropanyl chloride; addition;
- 【文献出处】 化学反应工程与工艺 ,Chemical Reaction Engineering and Technology , 编辑部邮箱 ,2006年02期
- 【分类号】TQ251.2
- 【被引频次】3
- 【下载频次】298