Sodium Chloride → 2-Bromo-1-(2,4-difluorophenoxy)-4-nitrobenzene

温度

110 °C

2-Bromo-1-fluoro-4-nitrobenzene (15 g, 68.2 mmol), 2,4-difluorophenol (7.82 mL, 82 mmol), and cesium carbonate (26.7 g, 82 mmol) were combined in DMSO (75 mL), heated at 110° C. for 1 hour, and then cooled. To the cooled reaction mixture was added water (1000 mL) and saturated aqueous sodium chloride (1000 mL). The mixture was extracted with ethyl acetate (3×200 mL). The combined organics were washed with saturated aqueous sodium chloride, dried (anhydrous magnesium sulfate), filtered, and concentrated under reduced pressure to give a crude solid which was used in the next step without additional purification.

1. temperaturecooled
2. customTo the cooled reaction mixture
3. extractionThe mixture was extracted with ethyl acetate (3×200 mL)
4. washThe combined organics were washed with saturated aqueous sodium chloride
5. dry with materialdried (anhydrous magnesium sulfate)
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure
8. customto give a crude solid which
9. customwas used in the next step without additional purification

ORDレコード

ord-de216df35a7543ff9ad64d58062f1a33

出典データセット

uspto-grants-2016_08

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09428514B2