反应详情

温度

110 °C

To a solution of 2,4-dichloro-6-(3-cyclopropyl-1-methyl-1H-pyrazol-5-yl)-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidine (0.110 g, 0.325 mmol) in DMA (2.2 mL) was added (R)-3-methylmorpholine (49.3 mg, 0.488 mmol) and DIPEA (284 μL, 1.63 mmol). The mixture was heated at 110° C. for 2 h. Water was added and the aqueous phase was extracted with EtOAc (3×). The organic phases were combined, washed with brine (3×), dried with sodium sulfate, filtered and concentrated under reduce pressure. Purification by FCC (0-60% EtOAc/heptane) provided the title compound (R)-4-(2-chloro-6-(3-cyclopropyl-1-ethyl-1H-pyrazol-5-yl)-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidin-4-yl)-3-methylmorpholine. MS (ESI+) m/z 403.1 (M+H)+.

1. extractionthe aqueous phase was extracted with EtOAc (3×)
2. washwashed with brine (3×)
3. dry with materialdried with sodium sulfate
4. filtrationfiltered
5. concentrationconcentrated
6. customPurification by FCC (0-60% EtOAc/heptane)