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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

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【作者】 赵贵财徐刚吴坚平杨立荣

【Author】 Zhao Guicai Xu Gang Wu Jianping Yang Lirong (Institute of Biochemical Engineering,College of Material Science and Chemical Engineering,Zhejiang University,Hangzhou 310027,China)

【机构】 浙江大学材化学院生物工程研究所浙江大学材化学院生物工程研究所 浙江杭州310027浙江杭州310027

【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.

  • 【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
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