반응 #3114

반응 방정식

4-Nitrophenol

sodium chlorodifluoroacetate

sodium hydroxide

→

title compound

수율 73.4%

4-difluoromethoxynitrobenzene

수율 73.4%

용매

DMF

water

반응 조건

후처리

1. 1
   온도the mixture was cooled to RT
2. 2
   추출was extracted twice with ether
3. 3
   세척The combined organic extracts were washed twice with brine
4. 4
   건조were dried (MgSO4)
5. 5
   여과filtered
6. 6
   기타evaporated
7. 7
   기타The residue was purified by flash chromatography (silica gel, 25% ethyl acetate/hexanes )

실험 절차

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.

출처