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) is heated at 40° C. for 24 h. The solvent is removed in vacuo. The resulting residue is partitioned between EtOAc (350 mL) and water (100 mL). The EtOAc layer is washed with water (3×), saturated aqueous NaCl (1×), dried over Na2SO4, and concentrated in vacuo. The resulting crude product is sonicated in Et2O (200 mL) and the resulting precipitate collected by filtration. This powder is 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 is removed in vacuo
2. customThe resulting residue is partitioned between EtOAc (350 mL) and water (100 mL)
3. washThe EtOAc layer is washed with water (3×), saturated aqueous NaCl (1×)
4. dry with materialdried over Na2SO4
5. concentrationconcentrated in vacuo
6. customThe resulting crude product is sonicated in Et2O (200 mL)
7. filtrationthe resulting precipitate collected by filtration
8. washThis powder is further washed with Et2O