methyl 5-amino-2-(difluoromethoxy)benzoate

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: Acetylchloride (1.8 mL, 25.3 mmol) in 25 mL THF was added to a mixture of methyl 5-amino-2-difluoromethoxy-benzoate (5.40 g, 24.9 mmol) with TEA (4.5 mL, 32.4 mmol) in 50 mL THF and the resulting mixture stirred for 15 min at ambient temperature. The mixture was filtered and the filtrate concentrated i. vac. The residue was mixed with acetonitrile and water, concentrated i. vac. and the solid filtered off. It was washed with water and dried at 40° C. The mixture was filtered the filtrate concentrated i The residue was mixed with acetonitrile and water concentrated i and the solid filtered off It was washed with water dried at 40° C.

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: Acetylchloride (1.8 mL, 25.3 mmol) in 25 mL THF was added to a mixture of methyl 5-amino-2-difluoromethoxy-benzoate (5.40 g, 24.9 mmol) with TEA (4.5 mL, 32.4 mmol) in 50 mL THF and the resulting mixture stirred for 15 min at ambient temperature. The mixture was filtered and the filtrate concentrated i. vac. The residue was mixed with acetonitrile and water, concentrated i. vac. and the solid filtered off. It was washed with water and dried at 40° C. The mixture was filtered the filtrate concentrated i The residue was mixed with acetonitrile and water concentrated i and the solid filtered off It was washed with water dried at 40° C.