تفاعل #3114

معادلة التفاعل

4-Nitrophenol

sodium chlorodifluoroacetate

sodium hydroxide

→

title compound

المردود 73.4%

4-difluoromethoxynitrobenzene

المردود 73.4%

المذيبات

DMF

water

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةthe mixture was cooled to RT
2. 2
   استخلاصwas extracted twice with ether
3. 3
   غسيلThe combined organic extracts were washed twice with brine
4. 4
   تجفيفwere dried (MgSO4)
5. 5
   ترشيحfiltered
6. 6
   أخرىevaporated
7. 7
   أخرىThe residue was purified by flash chromatography (silica gel, 25% ethyl acetate/hexanes )

الإجراء التجريبي

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.

المصدر