反应详情

温度

70 °C

A mixture of 1-(4-chloro-5H-pyrrolo[3,2-d]pyrimidin-7-yl)-2,2,2-trifluoro-1-[1-(4-fluorophenyl)-1H-indazol-5-yl]ethanol (43 mg, 0.09 mmol) and 1 mL of trifluoroacetic acid in 1 mL of water and 2 mL of dioxane was warmed at 70° C. After 18 hours, the reaction was diluted with saturated NaHCO3 and extracted with EtOAc. The combined organic layers were dried, filtered, and concentrated in vacuo. The residue was dissolved in 1 mL of DMF and purified by reverse phase HPLC (5-95% CH3CN/water+0.1% TFA). The desired fractions were combined and the CH3CN was removed in vacuo. The aqueous layer was made basic with saturated sodium bicarbonate and extracted with EtOAc. The combined organics were dried, filtered, and concentrated in vacuo to provide 18 mg (44%) of the title compound as a white solid. MS m/z 444.27 (MH+).

1. extractionextracted with EtOAc
2. customThe combined organic layers were dried
3. filtrationfiltered
4. concentrationconcentrated in vacuo
5. dissolutionThe residue was dissolved in 1 mL of DMF
6. custompurified by reverse phase HPLC (5-95% CH3CN/water+0.1% TFA)
7. customthe CH3CN was removed in vacuo
8. extractionextracted with EtOAc
9. customThe combined organics were dried
10. filtrationfiltered
11. concentrationconcentrated in vacuo