Dimethylformamide → 2,5-Difluoro-4-methoxybenzaldehyde

Temperatur

-78 °C

To a 250 mL three RB flask fitted with magnetic stirrer was charged 1-Bromo-2,5-difluoro-4-methoxybenzene (1.0 g, 4.5 mmol) in 10 mL of THF, cooled −78° C. To the stirred solvent was added n-butyl lithium (3.09 mL, 1.6M solution, 4.95 mmol) drop wise and stirred at same temperature, was added DMF (0.375 g, 5.13 mmol), once the temperature to reached room temperature and stirred about 16 h. Then reaction mixture was quenched with ice-cold water and extracted with ethyl acetate. The organic layer was washed with water, dried over anhydrous Na2SO4. The removal of solvent under reduced pressure to obtain liquid product (0.77 g, yield: 100.0%).

1. customto reached room temperature
2. stirringstirred about 16 h
3. customThen reaction mixture
4. customwas quenched with ice-cold water
5. extractionextracted with ethyl acetate
6. washThe organic layer was washed with water
7. dry with materialdried over anhydrous Na2SO4
8. customThe removal of solvent under reduced pressure

ORD-Eintrag

ord-7cfca20889a0403f907ed93675420ff1

Quelldatensatz

uspto-grants-2016_03

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09278915B2