Hydrochloric Acid → HCID 59228900, compound

Participants

Reaction Conditions

Reaction Steps

200 mL of dichloromethane was poured into a 1 L three-necked flask equipped with a stirrer, thermometer, dropping funnel, and nitrogen inlet tube, cooled to 0° C. using a salt-ice bath, and then 80.4 g (0.6 mol) of aluminum chloride and 40.3 g (0.6 mol) of pyrrole were added. Next, 104.7 g (0.50 mol) of 2,5-dichlorobenzoyl chloride dissolved in 100 mL of dichloromethane was slowly added dropwise using a dropping funnel. After completing the addition, the reactant was stirred for 3 hours while maintained at 5° C. to 10° C. using the salt-ice bath. After confirming the disappearance of raw materials by way of thin-layer chromatography, the reaction liquid was gradually added to 1 L of 2 N HCl, and excessive aluminum chloride was dissolved and removed. The organic layer was washed using 5% sodium bicarbonate water, water, and a sodium chloride solution, and the organic layer was dried using magnesium sulfate, and then the solvent was removed by an evaporator. The approximate yield amount was 120 g. The crude product was recrystallized from hexane/ethyl acetate to obtain the intended product in an amount of 95 g and at a yield of 79% as a milky white solid.

Provenance & Evidence