1-Bromo-3-(difluoromethyl)-5-nitrobenzene → 3-Bromo-5-(difluoromethyl)aniline

Temperatur

80 °C

1-Bromo-3-(difluoromethyl)-5-nitrobenzene (944 mg, 3.60 mmol) was treated with iron powder (804 mg, 23.43 mmol) in a mixture of acetic acid (1.35 ml) and ethanol (25 ml) and stirred at 80° C. for 3 h. The crude was filtered over Celite and the solvent was removed in vacuum. A mixture of a solution of sodium bicarbonate 4% and ethyl acetate was added and the resulting mixture was filtered over Celite. The organic phase was washed with water and brine, dried over magnesium sulphate and the solvent was remove to give 855 mg (100% yield) of the title compound as a dark solid, that was used in the next step without further purification. Purity 96%.

1. filtrationThe crude was filtered over Celite
2. customthe solvent was removed in vacuum
3. additionA mixture of a solution of sodium bicarbonate 4% and ethyl acetate
4. additionwas added
5. filtrationthe resulting mixture was filtered over Celite
6. washThe organic phase was washed with water and brine
7. dry with materialdried over magnesium sulphate
8. customthe solvent was remove

ORD-Eintrag

ord-c4cff1913b6f4f5f87b005f05641e7c6

Quelldatensatz

uspto-grants-2016_07

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09388189B2