反应详情

温度

80 °C

A mixture of 2,6-dichloro-9H-purine (5.2 g, 27.51 mmol), (S)-3-methylmorpholine (3.30 g, 32.62 mmol) and DIPEA (5.0 mL, 28.71 mmol) in IMS (130 mL) were heated at 80° C. for 3 h then stirred at r.t. for 17 h. The resulting white precipitate was collected by filtration and the filtrate concentrated in vacuo to a reduced volume and the resulting precipitate also collected by filtration. Both batches of solid were combined in DCM and the organic phase washed with H2O and brine, then dried (MgSO4) and concentrated in vacuo affording the title compound as a white powder (5.3 g, 76%). LCMS (method H): RT 2.54 min [M+H]+ 254.1

1. filtrationThe resulting white precipitate was collected by filtration
2. concentrationthe filtrate concentrated in vacuo to a reduced volume
3. filtrationthe resulting precipitate also collected by filtration
4. washthe organic phase washed with H2O and brine
5. dry with materialdried (MgSO4)
6. concentrationconcentrated in vacuo