反应详情

The mixture of tert-butyl cis-2-[(4-hydroxytetrahydro-2H-pyran-4-yl)methyl]-5-{[(1-isopropyl-1H-indazol-3-yl)carbonyl]amino}piperidine-1-carboxylate (292 mg, 0.583 mmol, step 6 of Example 2) and 10% hydrochloric acid in methanol (3 mL) was stirred at room temperature for 20 h. The mixture was concentrated under reduced pressure and the resulting residue was dissolved in dichloromethane/methanol (10/1, 10 mL). The solution was filtered through amine-silica gel washing with dichloromethane/methanol (10/1, 200 mL). The filtrate was concentrated under reduced pressure and the resulting residue was chromatographed on a column of silica gel eluting with dichloromethane/methanol/25% ammonium hydroxide (10:1:0.2) to give 249 mg (99%) of the title compound as a white crystal.

1. concentrationThe mixture was concentrated under reduced pressure
2. dissolutionthe resulting residue was dissolved in dichloromethane/methanol (10/1, 10 mL)
3. filtrationThe solution was filtered through amine-silica gel washing with dichloromethane/methanol (10/1, 200 mL)
4. concentrationThe filtrate was concentrated under reduced pressure
5. customthe resulting residue was chromatographed on a column of silica gel eluting with dichloromethane/methanol/25% ammonium hydroxide (10:1:0.2)