Methyl iodide → 4-Bromo-2,5-difluoroanisole

Temperature

45 °C

To a 100 mL RB flask fitted with magnetic stirrer was charged with 20 mL of DMF. To the stirred solvent were added 4-Bromo-2,5-difluorophenol (2.0 g, 9.6 mmol), K2CO3 (3.98 g, 28.8 mmol) and methyl iodide (1.63 g, 11.53 mmol), stirred at 45° C. for 15 minutes under nitrogen atmosphere. The RM was quenched with water, extracted with ethyl acetate (100 mL). The organic layer was washed with water (50 mL) and saturated brine solution (50 mL). The organic layer was dried over anhydrous Na2SO4 and the solvent was removed under reduced pressure. The product was obtained as white color solid (1.2 g, yield: 56.07%).

1. customTo a 100 mL RB flask fitted with magnetic stirrer
2. customThe RM was quenched with water
3. extractionextracted with ethyl acetate (100 mL)
4. washThe organic layer was washed with water (50 mL) and saturated brine solution (50 mL)
5. dry with materialThe organic layer was dried over anhydrous Na2SO4
6. customthe solvent was removed under reduced pressure

ORD record

ord-c5a2855b65414b28b37881dc4d1eb355

Source dataset

uspto-grants-2016_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09278915B2