2-Bromo-1-(2,4-dichlorophenyl)ethan-1-one → HCID 178477951, compound

Participants

Reaction Conditions

Reaction Steps

A suspension of 39.8 g (0.254 mol) of benzamidine hydrochloride and 13.7 g (0.254 mol) of sodium methylate in 170 ml of tetrahydrofuran was heated under reflux for 1 hour, and cooled to 25° C. A solution of 68.0 g (0.254 mol) of the above-mentioned crude 2-bromo-2′,4′-dichloroacetophenone in 120 ml of tetrahydrofuran was added dropwise in such a manner that the reaction temperature did not exceed 30° C. After the addition was complete, 13.7 g (0.254 mol) of sodium methylate was added, and the mixture was heated under reflux for 1 hour. Subsequently, the reaction solution was cooled to room temperature, and insolubles were filtered off. The filtrate was evaporated to dryness under reduced pressure to recover a solid. The solid was successively washed with water and toluene and then dried, to give 33.8 g (46.0% crude yield) of crude crystals of the desired product. The crude crystals were recrystallized using acetonitrile to give pale yellow purified crystals.

Provenance & Evidence