反应详情

温度

110 °C

In a sealed tube, (4-Isopropoxy-phenyl)-(7H-pyrrolo[2,3-d]pyrimidin-2-yl)-amine (350 mg, 1.17 mmol), 4-bromophenylmethylsulfone (552 mg, 2.35 mmol), CuI (68.4 mg, 0.352 mmol), and K3PO4 (763 mg, 3.52 mmol) are suspended in 1,4-dioxane (10 mL). Then, trans-1,2-diaminocyclohexane (42.7 μL, 0.352 mmol) is added at rt. The reaction vial is flushed with Ar and the mixture is heated to 110° C. for 6 h. After cooling to rt, the reaction mixture is diluted with EtOAc and the organic layer is washed with saturated aqueous NaCl solution (3×). The organic layer is dried over Na2SO4, filtered, and concentrated under reduced pressure. The residue is purified by reverse phase prep-HPLC (Waters) to afford the title compound (3) as an off-white solid. HPLC: tR=1.67 min (Method A); MS-ES: (M+H)+=423.

1. customThe reaction
2. customvial is flushed with Ar
3. temperatureAfter cooling to rt
4. additionthe reaction mixture is diluted with EtOAc
5. washthe organic layer is washed with saturated aqueous NaCl solution (3×)
6. dry with materialThe organic layer is dried over Na2SO4
7. filtrationfiltered
8. concentrationconcentrated under reduced pressure
9. customThe residue is purified by reverse phase prep-HPLC (Waters)