反应详情

To the solution of tert-butyl(trans-3-(1H-pyrrolo[2,3-b]pyridin-1-yl)cyclobutyl)carbamate (294 mg, 1.02 mmol) in DCM (2.0 ml) was added trifluoroacetic acid, 99% (760 μl, 10.2 mmol). The reaction mixture was stirred at room temperature under N2 for 1 h. The solvent was evaporated and the residue was triturated with DCM three times, redissolved in DCM, and then treated with solid NaHCO3. The solid was filtered off and the filtrate concentrated in vacuo. The crude material was purified by chromatography through a Redi-Sep pre-packed silica gel column (12 g), eluting with a gradient of 0% to 100% EtOAc in hexane, then 15% MeOH in EtOAc, to provide trans-3-(1H-pyrrolo[2,3-b]pyridin-1-yl)cyclobutanamine (75 mg, 0.401 mmol, 39.2% yield) as light-yellow oil. ESI (M+1) 188.0.

1. customThe solvent was evaporated
2. customthe residue was triturated with DCM three times
3. dissolutionredissolved in DCM
4. additiontreated with solid NaHCO3
5. filtrationThe solid was filtered off
6. concentrationthe filtrate concentrated in vacuo
7. customThe crude material was purified by chromatography through a Redi-Sep pre-packed silica gel column (12 g)
8. washeluting with a gradient of 0% to 100% EtOAc in hexane