反应详情

温度

40 °C

A mixture of 5-methyl-1H-pyrazol-3-amine (3.00 g, 30.9 mmol), 2,4-dichloro-5-methylpyrimidine (5.03 g, 30.9 mmol, 1 equiv.) and Na2CO3 (3.60 g, 34.0 mmol, 1.1 equiv.) in EtOH (100 mL) was heated at 40° C. for 24 h. The solvent was removed in vacuo. The resulting residue was partitioned between EtOAc (350 mL) and water (100 mL). The EtOAc layer was washed with water (3×), saturated aqueous NaCl (1×), dried over Na2SO4, and concentrated in vacuo. The resulting crude product was sonicated in Et2O (200 mL) and the resulting precipitate collected by filtration. This powder was further washed with Et2O, providing the product 2-chloro-5-methyl-N-(5-methyl-1H-pyrazol-3-yl)pyrimidin-4-amine; ESMS m/z 224.1 (M+H+).

1. customThe solvent was removed in vacuo
2. customThe resulting residue was partitioned between EtOAc (350 mL) and water (100 mL)
3. washThe EtOAc layer was washed with water (3×), saturated aqueous NaCl (1×)
4. dry with materialdried over Na2SO4
5. concentrationconcentrated in vacuo
6. customThe resulting crude product was sonicated in Et2O (200 mL)
7. filtrationthe resulting precipitate collected by filtration
8. washThis powder was further washed with Et2O