反应详情

温度

110 °C

To the mixture of 2-chloro-6-methyl-N-(1H-pyrazol-5-yl)pyrimidin-4-amine prepared in Referential Example 1 (25.5 mg) and (R)-3-(tert-butoxycarbonylamino)piperidine (50.9 mg) in DMSO (5 ml) was added DIEA (210.0 μL). And the mixture was heated to 110° C. under stirring for overnight. The resulting mixture was cooled to room temperature, poured into brine and extracted with EtOAc. The extract was washed with saturated aqueous solution of NaHCO3, dried over Na2SO4 and concentrated in vacuo. And the residue was purified with silica gel column chromatography (eluent: hexane/EtOAc=99/1˜0/100) to give tert-butyl {(3R)-1-[4-methyl-6-(1H-pyrazol-5-ylamino)pyrimidin-2-yl]piperidin-3-yl}carbamate (26.0 mg) as a pale yellow solid.

1. temperatureThe resulting mixture was cooled to room temperature
2. extractionextracted with EtOAc
3. washThe extract was washed with saturated aqueous solution of NaHCO3
4. dry with materialdried over Na2SO4
5. concentrationconcentrated in vacuo
6. customAnd the residue was purified with silica gel column chromatography (eluent: hexane/EtOAc=99/1˜0/100)