反应详情

3-({[1-(4-Hydroxy-4-thiazol-2-yl-cyclohexyl)-azetidin-3-ylcarbamoyl]-methyl}-amino)-5-trifluoromethyl-indazole-1-carboxylic acid tert-butylamide (as prepared in Example 80, 150 mg, 0.25 mmol) in TFA (2 mL) in a sealed tube was heated at 80° C. for 6 hours. The TFA was removed, and the residue was partitioned between DCM and saturated NaHCO3. The organic layer was washed with brine, dried over anhydrous Na2SO4, filtered and concentrated to give the crude material, purified by silica gel column (DCM: 7 N NH3 in MeOH 9:1) to afford the title compound as white solid (36 mg, 27%).

1. customThe TFA was removed
2. customthe residue was partitioned between DCM and saturated NaHCO3
3. washThe organic layer was washed with brine
4. dry with materialdried over anhydrous Na2SO4
5. filtrationfiltered
6. concentrationconcentrated
7. customto give the crude material
8. custompurified by silica gel column (DCM: 7 N NH3 in MeOH 9:1)