反应详情

To a solution of N-hydroxy-1-(1-methyl-1H-imidazol-5-yl)-1-phenylmethanimine (3.90 g, 19.4 mmol) and 2-(chloromethyl)pyrimidin-4-amine (3.06 g, 21.3 mmol) in acetonitrile (50 mL) were added cesium carbonate (13.3 g, 40.7 mmol) and potassium iodide (322 mg, 1.93 mmol). After stirring at room temperature for 29 h, N-N-dimethylformamide (5 mL) was added and the mixture was further at room temperature for 72 h. The reaction mixture was filtered, the insolubles washed with acetone, and the filtrate concentrated in vacuo. Purification on silica gel afforded 2-[({[(1-methyl-1H-imidazol-5-yl)(phenyl)methylene]amino}oxy)methyl]pyrimidin-4-amine [3.61 g, yield 16%; HPLC/MS: m/z=309 (M+H); log P(HCOOH)<0.23].

1. waitthe mixture was further at room temperature for 72 h
2. filtrationThe reaction mixture was filtered
3. washthe insolubles washed with acetone
4. concentrationthe filtrate concentrated in vacuo
5. customPurification on silica gel