反应详情

温度

100 °C

To a 100-mL round-bottomed flask was added 1,1,1,3,3,3-hexafluoro-2-(4-(2-((2-methoxy-4-pyridinyl)methyl)-4-(2-thiophenylsulfonyl)-1-piperazinyl)phenyl)-2-propanol (72 mg, 0.12 mmol), 5N hydrochloric acid (0.121 mL, 0.60 mmol), and dioxane (3 mL). The reaction mixture was stirred at 100° C. for 16 h and allowed to cool to room temperature. The reaction mixture was diluted with saturated NaHCO3 (20 mL) and extracted with EtOAc (2×40 mL). The organic extract was washed with saturated NaCl (5 mL) and dried over Na2SO4. The solution was filtered and concentrated in vacuo to give the crude material as an off-white solid. The crude product was purified by silica gel chromatography, eluting with 5% MeOH/EtOAc to give 4-((4-(2-thiophenylsulfonyl)-1-(4-(2,2,2-trifluoro-1-hydroxy-1-(trifluoromethyl)ethyl)phenyl)-2-piperazinyl)methyl)-2(1H)-pyridinone (58 mg) as a white solid.

1. temperatureto cool to room temperature
2. extractionextracted with EtOAc (2×40 mL)
3. extractionThe organic extract
4. washwas washed with saturated NaCl (5 mL)
5. dry with materialdried over Na2SO4
6. filtrationThe solution was filtered
7. concentrationconcentrated in vacuo
8. customto give the crude material as an off-white solid
9. customThe crude product was purified by silica gel chromatography
10. washeluting with 5% MeOH/EtOAc