2-CHLORO-3,6-DIFLUOROBENZAMIDE synthesis

Yield:-

Reaction Conditions:

Stage #1: 2-chloro-3,6-difluorobenzamidewith trichlorophosphate at 95; for 2 h;
Stage #2: with potassium carbonate in water;ethyl acetate;

Steps:

2-ChIoro-3,6-difluorobenzoαitriIe2-Chloro-3,6-difluorobenzamide (0.80 g, 4.18 mmol) in POCl₃ (12 mL) was heated for 2 h at 95 ⁰C. The sol. was cooled and the excess of POCl₃ was removed by distillation under reduced pressure. The residue was diluted with EtOAc and aq. 10% K₂CO₃ was cautiously added. The layers were separated and the org. phase was washed with water (2x), and brine. The org. extracts were dried over MgSO₄, filtered, and the solvent were removed under reduced pressure to yield the title compound (0.46 g) that was not further purified.

References:

WO2006/63610,2006,A1 Location in patent:Page/Page column 15