2',5'-difluoro-4'-methoxyacetophenone synthesis

Yield:-

Reaction Conditions:

in tetrahydrofuran at 0 - 20; for 1.5 h;Inert atmosphere;

Steps:

207

2,5-Difluoro-4-methoxyacetophenone The compound of Example 206 (1.50 g) was dissolved in THF (30 mL) under an argon atmosphere, and methyl magnesium bromide (0.84 mol/L THF solution, 17.0 mL) was added thereto at 0°C, followed by stirring at room temperature for 1.5 hours. To the reaction liquid was added a saturated aqueous ammonium chloride solution, followed by extraction with ethyl acetate, and the extracted layer was washed with saturated brine and then dried over anhydrous sodium sulfate. After evaporating the solvent under reduced pressure, the residue was purified by silica gel chromatography (hexane:ethyl acetate=4:1) to obtain the desired product (1.12 g) as a white powder. ¹H NMR (CDCl₃, 400 MHz): δ 2.60 (3H, d, J=5.5 Hz), 3.94 (3H, s), 6.70 (1H, dd, J=11.6, 6.7 Hz), 7.64 (1H, dd, J=11.6, 6.7 Hz).

References:

EP2168959,2010,A1 Location in patent:Page/Page column 174