تفاعل #3116

معادلة التفاعل

ethyl acetate

4-Nitrophenol

methyl chlorodifluoroacetate

potassium carbonate

→

title compound

المردود 65.0%

4-difluoromethoxynitrobenzene

المردود 65.0%

المذيبات

DMF

ظروف التفاعل

المعالجة

1. 1
   غسيلthe organic layer was washed three times with 10% NaOH
2. 2
   استخلاصThe organic extract
3. 3
   تجفيفwas dried (MgSO4)
4. 4
   ترشيحfiltered
5. 5
   أخرىevaporated
6. 6
   أخرىThe residue was purified by flash chromatography (silica gel, 20% ether/hexanes)

الإجراء التجريبي

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.

المصدر