4-Nitrophenol → 4-(Difluoromethoxy)nitrobenzene

Temperatur

125 °C

4-Nitrophenol (0.10 g, 0.72 mmol, Aldrich), sodium chlorodifluoroacetate (0.11 g, 0.72 mmol, Alfa Products) and sodium hydroxide (0.03 g, 0.72 mmol) were combined in dry DMF (1 mL) under an atmosphere of argon. After stirring at 125° C. for 1 h, the mixture was cooled to RT, was diluted with water and was extracted twice with ether. The combined organic extracts were washed twice with brine, were dried (MgSO4), filtered and evaporated. The residue was purified by flash chromatography (silica gel, 25% ethyl acetate/hexanes ) to provide the title compound as a white solid (0.10 g, 73%). mp 33°-35° C.

1. temperaturethe mixture was cooled to RT
2. extractionwas extracted twice with ether
3. washThe combined organic extracts were washed twice with brine
4. dry with materialwere dried (MgSO4)
5. filtrationfiltered
6. customevaporated
7. customThe residue was purified by flash chromatography (silica gel, 25% ethyl acetate/hexanes )

ORD-Eintrag

ord-b2d252a75b1947e3893ae5090ef4d0e4

Quelldatensatz

uspto-grants-1998_03

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US05731477