反応 #3116

反応方程式

ethyl acetate

4-Nitrophenol

methyl chlorodifluoroacetate

potassium carbonate

→

title compound

収率 65.0%

4-difluoromethoxynitrobenzene

収率 65.0%

溶媒

DMF

反応条件

後処理

1. 1
   洗浄the organic layer was washed three times with 10% NaOH
2. 2
   抽出The organic extract
3. 3
   乾燥was dried (MgSO4)
4. 4
   ろ過filtered
5. 5
   その他evaporated
6. 6
   その他The residue was purified by flash chromatography (silica gel, 20% ether/hexanes)

実験手順

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.

出典