반응 #3116

반응 방정식

ethyl acetate

4-Nitrophenol

methyl chlorodifluoroacetate

potassium carbonate

→

title compound

수율 65.0%

4-difluoromethoxynitrobenzene

수율 65.0%

용매

DMF

반응 조건

후처리

1. 1
   세척the organic layer was washed three times with 10% NaOH
2. 2
   추출The organic extract
3. 3
   건조was dried (MgSO4)
4. 4
   여과filtered
5. 5
   기타evaporated
6. 6
   기타The residue was purified by flash chromatography (silica gel, 20% ether/hexanes)

실험 절차

4-Nitrophenol (0.14 g, 1.0 mmol, Aldrich), methyl chlorodifluoroacetate (0.29 g, 2.0 mmol, Aldrich) and potassium carbonate (0.29 g, 2.1 mmol) were combined in dry DMF (0.5 mL) under an argon atmosphere. After stirring at 95°-100° C. for 0.5 h, the mixture was cooled to RT, ethyl acetate (20 mL) was added and the organic layer was washed three times with 10% NaOH. The organic extract was dried (MgSO4), filtered and evaporated. The residue was purified by flash chromatography (silica gel, 20% ether/hexanes) to provide the title compound as a white solid (0.12 g, 65%). mp 33°-35° C.

출처