反应详情

To solution of (3S)-3-[[2-[5-chloro-1-(p-tolylsulfonyl)pyrrolo[2,3-b]pyridin-3-yl]-5-fluoro-pyrimidin-4-yl]amino]cyclohexanone (0.41 g, 0.81 mmol) in EtOH (8.2 mL) was added hydroxylamine hydrochloride (0.11 g, 1.61 mmol). The reaction mixture was stirred at room temperature overnight. Then the mixture was warmed to 70° C. for 15 min. The reaction mixture was concentrated in vacuo, suspended in EtOAc-DCM, washed with half saturated brine (2×) and filtered through a SiO2 plug. The resulting residue was azeotroped with CH3CN (2×) to provide an off white powder which was used without further purification.

1. temperatureThen the mixture was warmed to 70° C. for 15 min
2. concentrationThe reaction mixture was concentrated in vacuo
3. washwashed with half saturated brine (2×)
4. filtrationfiltered through a SiO2 plug
5. customThe resulting residue was azeotroped with CH3CN (2×)
6. customto provide an off white powder which
7. customwas used without further purification