反应详情

温度

100 °C

To a 20-mL vial, 3-(1-methylethyl)-4-(((2S)-4-((5-nitro-2-thiophenyl)sulfonyl)-2-piperazinyl)methyl)-2-piperazinone (262 mg, 0.607 mmol), 2-(2-chloropyrimidin-5-yl)-1,1,1,3,3,3-hexafluoropropan-2-ol (170 mg, 0.607 mmol, Intermediate D) and Hünig's base (323 μL, 1.852 mmol) were dissolved into dioxane (3.77 mL). The vial was sealed and the reaction mixture was stirred at 100° C. for 12 h. After cooling to room temperature, the mixture was partitioned between water and EtOAc. The aqueous phase was extracted with EtOAc, and the combined organic phases were washed with brine. The organic phase was dried (Na2SO4), filtered and concentrated in vacuo. The crude residue was purified by silica gel chromatography (40 to 100% EtOAc in hexanes gradient) to give the title compound (228 mg).

1. customThe vial was sealed
2. temperatureAfter cooling to room temperature
3. customthe mixture was partitioned between water and EtOAc
4. extractionThe aqueous phase was extracted with EtOAc
5. washthe combined organic phases were washed with brine
6. dry with materialThe organic phase was dried (Na2SO4)
7. filtrationfiltered
8. concentrationconcentrated in vacuo
9. customThe crude residue was purified by silica gel chromatography (40 to 100% EtOAc in hexanes gradient)