反应详情

温度

85 °C

A solution of tert-butyl 1-(5-(5-(2,6-difluorophenyl)-1-(tetrahydro-2H-pyran-2-yl)-1H-indazol-3-yl)pyridin-3-yl)piperidin-4-ylcarbamate (120 mg, 0.204 mmol) in dioxane (5 mL) was treated with concentrated HCl (0.113 mL, 2.035 mmol). The reaction was heated to 85° C. After 1 h, the reaction was cooled to 23° C. and concentrated. The residue (as HCl salt) was free-based using a Silicycle Si-propylsulfonic acid ion exchange column (catalog # R51230B). The compound was diluted in MeOH and added to a pad of the resin (wetted and flushed with 10 mL MeOH). It was flushed with MeOH (50 mL), and then the product was “released” using 2.0 M NH3 in MeOH solution (50 ml). The final filtrate was concentrated, affording 1-(5-(5-(2,6-difluorophenyl)-1H-indazol-3-yl)pyridin-3-yl)piperidin-4-amine. MS (ESI, pos. ion) m/z: 406.2 (M+1).

1. temperaturethe reaction was cooled to 23° C.
2. concentrationconcentrated
3. additionThe compound was diluted in MeOH
4. additionadded to a pad of the resin (wetted and flushed with 10 mL MeOH)
5. customIt was flushed with MeOH (50 mL)
6. concentrationThe final filtrate was concentrated