5-氯-2,3-二氢-1-茚酮的合成研究

以3-氯丙酰氯、氯苯、三氯化铝、浓硫酸为原料合成5-氯-2,3-二氢-1-茚酮,对影响反应的主要因素进行了研究,优化了条件,优化后的反应条件为:氯代酮合成:n(三氯化铝)∶n(氯苯)∶n(3-氯丙酰氯)=1.1∶4∶1,滴加温度为5℃,滴加时间2h,保温温度60℃,保温时间3h;5-氯茚酮合成:搅拌速度小于100r/min,n(H2SO4)∶n(氯代酮)=36.8∶1,滴加时间4h,溶剂为石油醚(90-120℃)。此工艺原料价廉易得,产品纯度高,总收率达50.6%,产品纯度达98%。

Synthesis of 5-Chloro-2,3-dihydro-1H-inden-1-one

5-Chloro-2,3-dihydro-1H-inden-1-one was synthesized from 3-chloropropionyl chloride,chlorobenzene,aluminium chloride and sulfuric acid, the major influences factors on this reactions were studied, the reaction condition was optimized. The optimum conditions: 3-ch-loro-1-(4-chlorphenyl)-1-propanone:n(aluminium chloride) ∶ n(chlorobenzene) ∶ n(3-chloropro-pionyl chloride)=1.1 ∶ 4 ∶ 1, drop temperature was 5 ℃,drop time was 2 h,the reaction proceeded 60 ℃ for 3 h;5-chloro-2,3-dihydro-1H-inden-1-one ∶ n(sulfuric acid) ∶ n(3-chloro-1-(4-chlorphenyl)-1-propanone)=36.8 ∶ 1, the stirring speed was under 100 r/min,drop time was 4 h,solvent was petroleum ether(90~120 ℃). The procedure was simple and high purity, the yield and purity of product was about 50.6% and 98%,respectively.