反应详情

温度

60 °C

A 2 L 3-neck round bottom flask equipped with a nitrogen bubbler, thermocouple, stir bar, heating mantle and condenser was charged with 4-[5-fluoro-2-(trifluoromethyl)phenyl]-4-{[4-(trifluoromethyl)phenyl]sulfonyl}cyclohexanol (94.7 g, 201 mmol) in THF (1 L). Trifluoromethanesulfonamide (45.0 g, 302 mmol) and triphenylphosphine (79 g, 302 mmol) were added, followed by DIAD (0.059 L, 302 mmol,) which was added dropwise over 20 min. The reaction was heated to 60° C. and stirred for 18 hrs at 60° C. The reaction was concentrated and dissolved in CH2Cl2 and purified by column chromatography on silica gel, eluting with ethyl acetate/heptanes to provide 1,1,1-trifluoro-N-(4-[5-fluoro-2-(trifluoromethyl)phenyl]-4-{[4-(trifluoromethyl)phenyl]sulfonyl}cyclohexyl)methanesulfonamide.

1. customA 2 L 3-neck round bottom flask equipped with a nitrogen bubbler
2. temperatureheating mantle
3. additionwas added dropwise over 20 min
4. stirringstirred for 18 hrs at 60° C
5. concentrationThe reaction was concentrated
6. dissolutiondissolved in CH2Cl2
7. custompurified by column chromatography on silica gel
8. washeluting with ethyl acetate/heptanes