Oxalyl chloride → 2,6-Difluorobenzoyl isocyanate

Participants

Reaction Conditions

Reaction Steps

0.25 g (1.6 mmol) of 2,6-difluorobenzamide and 0.22 g (1.8 mmol, 1.1 eq) of oxalyl chloride were added to 10 ml of 1,2-dichloroethane and then the mixture was stirred for 8 hours at 100° C. The reaction solution was cooled down to room temperature. The reaction solvent and excessive oxalyl chloride were removed by distillation under reduced pressure to obtain 2,6-difluorobenzoyl isocyanate in an oily state. 10 ml of fresh 1,2-dichloroethane and 0.3 g (1.6 mmol) of 2-chloro-4-fluoro-3-trifluoromethyl aniline were successively added thereto, reacted for 2 hours and filtered to obtain 0.45 g (Yield 73%) of the title compound as a solid.

Provenance & Evidence