Water → HCID 23298019, compound

Participants

Reaction Steps

A solution of 37.5 g (214 mmol) of 2-methyl-4-trifluoromethylaniline (DE 2750170 A1) and 44.7 ml (321 mmol) of triethylamine in 750 ml of ethyl acetate is cooled to +3° C. by means of an icebath. Ethyl oxalyl chloride (26.2 ml, 235.5 mmol) is slowly added dropwise so that the temperature does not rise above +10° C. The mixture is then stirred for a further 2 hours. The mixture is treated with water, washed with a 10% aqueous sodium hydrogencarbonate solution and with brine, dried over sodium sulfate and concentrated. Crystallization of the crude product affords 52.75 g of the title compound as white crystals.

Provenance & Evidence