反应详情

温度

110 °C

In a seal tube, 2-chloro-7H-pyrrolo[2,3-d]pyrimidine (600 mg, 3.56 mmol), 4-bromophenylmethylsulfone (700 mg, 4.10 mmol), CuI (239 mg, 1.23 mmol), and K3PO4 (2.67 g, 12.3 mmol) are suspended in 1,4-dioxane (30 mL). Then, trans-1,2-diaminocyclohexane (149 μL, 1.23 mmol) is added at rt. The reaction vial is flushed with Ar and the mixture is heated to 110° C. for 3 h. After cooling to rt, the reaction mixture is concentrated under reduce pressure. The residue is suspended in EtOAc and washed with saturated aqueous NaCl solution (3×). The organic layer is dried over MgSO4, filtered, and concentrated under reduced pressure. The solid residue is triturated with small amounts of EtOAc to yield the title compound as a brown solid.

1. customThe reaction
2. customvial is flushed with Ar
3. temperatureAfter cooling to rt
4. concentrationthe reaction mixture is concentrated
5. washwashed with saturated aqueous NaCl solution (3×)
6. dry with materialThe organic layer is dried over MgSO4
7. filtrationfiltered
8. concentrationconcentrated under reduced pressure
9. customThe solid residue is triturated with small amounts of EtOAc