Hydrochloric Acid → 1-Acetyl-4-(2',4'-difluorobenzoyl)piperidine

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Reaction Steps

1,3-difluorobenzene (6.7 g, 58.7 mmol) and ammonium chloride (13.3 g, 250 mmol) are added to 15 ml of dichloromethane and cooled to room temperature; thereto is drop-added 50 ml of dichloromethane wherein 1-acetyl-4-piperidinyl carboxylic acid chloride (9.8 g, 51.8 mmol) is dissolved. A reaction is carried out at reflux for 3 hours and the resulting mixture is poured into a mixture of ice and hydrochloric acid after completion of reaction. The mixture is extracted with dichloromethane (20 ml×3). The organic phase is separated, dried over anhydrous magnesium sulfate, filtered, and evaporated to dryness to obtain 5.01 g of a product, with a yield of 36%.

Provenance & Evidence