Water → 3-Chloro-6-fluoro-2-(trifluoromethyl)quinoxaline

Participants

Reaction Conditions

Reaction Steps

7-Fluoro-3-(trifluoromethyl)quinoxalin-2-ol (24.1 g) and POCl3 (158.1 g) were combined and warmed to 100° C. for 12 h. The reaction mixture was cooled to room temperature and diluted with acetonitrile (104 mL). To a separate vessel was charged water (320 g) and acetonitrile (124 g), then cooled to 10° C. The reaction mixture was added to the acetonitrile/water mixture over 1 hour. The slurry was cooled to 10° C. for 30 min, then it was filtered and the cake was washed with 2:1 (v/v) water:acetonitrile (3×65 mL). The solid was dried under vacuum at 50° C. for 14 h (24.7 g, 95% yield).

Provenance & Evidence