Реакция #3114

Уравнение реакции

4-Nitrophenol

sodium chlorodifluoroacetate

sodium hydroxide

→

title compound

Выход 73.4%

4-difluoromethoxynitrobenzene

Выход 73.4%

Растворители

DMF

water

Условия реакции

Обработка

1. 1
   Температураthe mixture was cooled to RT
2. 2
   Экстракцияwas extracted twice with ether
3. 3
   ПромывкаThe combined organic extracts were washed twice with brine
4. 4
   Сушкаwere dried (MgSO4)
5. 5
   Фильтрацияfiltered
6. 6
   Другоеevaporated
7. 7
   ДругоеThe residue was purified by flash chromatography (silica gel, 25% ethyl acetate/hexanes )

Методика

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.

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