42348-86-7

3946-29-0

42348-86-7

General procedure for the synthesis of 5-chloro-1-indanone from 3,4'-dichloropropiophenone: In an experimental setup equipped with a thermometer, a 500 mL four-necked flask, a stirrer, and a condensing device, 50 g of Et3NHCl-1.8AlCl3 ionic liquid (molar ratio 1.8) and 50 g of n-octane were added, and the temperature was raised to 70-80 °C. A solution consisting of 100 g of 3-chloro-1-(4-chlorophenyl)-1 -acetone and 100 g of n-octane was slowly added dropwise, followed by raising the temperature to 110-120 °C, and the reaction was kept at this temperature for 3-4 hours. The hydrogen chloride gas generated during the reaction was discharged through the top of the condenser tube and introduced into the suction tower for absorption. The reaction process was monitored by chromatography until 3-chloro-1-(4-chlorophenyl)-1-propanone was fully reacted. Upon completion of the reaction, the reaction mixture was transferred to a 1000 mL jacketed hydrolysis kettle and hydrolyzed by slowly adding 100 g of water under stirring. During the hydrolysis, the temperature was kept between 90-95 °C by circulating water cooling. Upon completion of hydrolysis, the stirring was stopped and the mixture was transferred to a separatory funnel and left to stratify. The separated n-octane phase enters the decolorization tank for conventional decolorization, and then the decolorized material is transferred to the crystallization kettle and cooled to 0-30°C for crystallization. The crystallization product was centrifuged and dried to obtain 72 g of finished 5-chloro-1-indanone product with a melting point of 92.6-93.5 °C and a yield of 72%.