反应详情

To 3-(3-ethyl-1-((6-methylpyridin-2-yl)methyl)-1H-indazol-4-ylcarbamoyl) imidazo[1,2-a]pyridine-7-carboxylic acid (26 mg, 0.057 mmol; prepared as in Example 28, step A) in DMF (2 mL) was added di(1H-imidazol-1-yl)methanone (14 mg, 0.086 mmol). The reaction mixture was stirred at ambient temperature for 1 hour. tert-Butyl 3-aminopyrrolidine-1-carboxylate (32 mg, 0.17 mmol) was added to the reaction mixture. The mixture was sealed and heated at 70° C. for 2 hours and cooled to ambient temperature. DMF was removed under reduced pressure. The residue was triturated with Et2O. The resulting tan solid was dissolved in DCM (1 mL). TFA (1 mL) was added to the DCM solution. The reaction mixture was stirred for 30 minutes and then concentrated under reduced pressure. The residue was purified by silica gel chromatography (DCM/MeOH/NH4OH 10:1:0.1) to provide the final product (10 mg). MS (ES+APCI) m/z=523 (M+H).

1. customThe mixture was sealed
2. temperatureheated at 70° C. for 2 hours
3. temperaturecooled to ambient temperature
4. customDMF was removed under reduced pressure
5. customThe residue was triturated with Et2O
6. dissolutionThe resulting tan solid was dissolved in DCM (1 mL)
7. additionTFA (1 mL) was added to the DCM solution
8. stirringThe reaction mixture was stirred for 30 minutes
9. concentrationconcentrated under reduced pressure
10. customThe residue was purified by silica gel chromatography (DCM/MeOH/NH4OH 10:1:0.1)