反应详情

温度

150 °C

A 20-mL microwave vial was charged with 2-(4-(4-((6-chloro-5-fluoro-3-pyridinyl)sulfonyl)-2-(1-propyn-1-yl)-1-piperazinyl)phenyl)-1,1,1,3,3,3-hexafluoro-2-propanol (165 mg, 0.30 mmol), aq. ammonium hydroxide (3 mL, 30% solution, 15.4 mmol, J. T. Baker, Phillipsburg, N.J.) and EtOH (3 mL). The is reaction vessel was sealed and the mixture heated to 150° C. overnight. The reaction was diluted with water (50 mL) and extracted with EtOAc (3×100 mL). The combined organics were dried (Na2SO4), filtered, and concentrated to give an oil that was purified via column chromatography on silica gel (0-10% MeOH in CH2Cl2) to give 2-(4-(4-((6-amino-5-fluoro-3-pyridinyl)sulfonyl)-2-(1-propyn-1-yl)-1-piperazinyl)phenyl)-1,1,1,3,3,3-hexafluoro-2-propanol (60 mg) as a mixture of two isomers.

1. customThe is reaction vessel
2. customwas sealed
3. extractionextracted with EtOAc (3×100 mL)
4. dry with materialThe combined organics were dried (Na2SO4)
5. filtrationfiltered
6. concentrationconcentrated
7. customto give an oil that
8. customwas purified via column chromatography on silica gel (0-10% MeOH in CH2Cl2)