反应详情

A mixture of 5-chloro-3-(3-chlorophenyl)pyrazolo[1,5-a]pyrimidine (100 mg, 0.379 mmol), (S)-piperidin-3-amine (76 mg, 0.757 mmol), and DIEA (0.158 ml, 1.515 mmol) in 2-propanol (3 ml) was irradiated to 150° C. for 14 h in a Biotage microwave. After cooling, the mixture was diluted with saturated aqueous NaHCO3, and extracted three times with EtOAc. The combined extracts were washed with brine, dried over Na2SO4 and concentrated in vacuo. After absorbing on celite, the compound was purified by chromatography (12 g silica, 0-15% methanol/DCM) to give (S)-1-(3-(3-chlorophenyl)pyrazolo[1,5-a]pyrimidin-5-yl)piperidin-3-amine (35 mg, 28% yield) as a white solid.

1. customwas irradiated to 150° C. for 14 h in a Biotage microwave
2. temperatureAfter cooling
3. extractionextracted three times with EtOAc
4. washThe combined extracts were washed with brine
5. dry with materialdried over Na2SO4
6. concentrationconcentrated in vacuo
7. customAfter absorbing on celite
8. customthe compound was purified by chromatography (12 g silica, 0-15% methanol/DCM)