반응 #493773

반응 방정식

sodium bicarbonate

α-(2,4-difluorophenyl)-5-(2,6-difluorophenyl)-1,3-dimethyl-1H-pyrazole-4-methanol

bis(2-methoxyethyl)aminosulfur trifluoride

→

title compound

5-(2,6-difluorophenyl)-4-[(2,4-difluorophenyl)fluoromethyl]-1,3-dimethyl-1H-pyrazole

용매

dichloromethane

반응 조건

후처리

1. 1
   온도cooled to −78° C.
2. 2
   추출The resulting mixture was extracted with dichloromethane (3×)
3. 3
   건조the combined organic layers were dried over magnesium sulfate
4. 4
   여과filtered
5. 5
   농축concentrated under reduced pressure
6. 6
   기타The resulting material was purified by MPLC (50% ethyl acetate in hexanes as eluant)

실험 절차

To a mixture of α-(2,4-difluorophenyl)-5-(2,6-difluorophenyl)-1,3-dimethyl-1H-pyrazole-4-methanol (i.e. the product of Example 4) (70 mg, 0.20 mmol) in dichloromethane (2 mL) at −78° C. was added bis(2-methoxyethyl)aminosulfur trifluoride (Deoxo-Fluor®) (40 μL, 0.24 mmol). The reaction mixture was stirred overnight at room temperature, and then cooled to −78° C. and saturated aqueous sodium bicarbonate solution (3 mL) was added dropwise. The resulting mixture was extracted with dichloromethane (3×) and the combined organic layers were dried over magnesium sulfate, filtered and concentrated under reduced pressure. The resulting material was purified by MPLC (50% ethyl acetate in hexanes as eluant) to provide the title compound, a compound of the present invention, as a solid (30 mg)

출처