反应详情

To a solution of 4,6-dichloropyrimidine (2.0 g, 13.4 mmol) in p-dioxane (50 mL), 3-amino-4,N-dimethyl-benzamide (3.0 g, 18.3 mmol) and DIEA (2.3 mL) were added. The resulting mixture was heated to reflux for 4 days. The solvent was removed in vacuo, the residue was taken in water and ethyl acetate, and the ethyl acetate layer was separated and concentrated. The product was purified by silica gel column chromatography using ethyl acetate:hexane (1:1) as eluent to afford the pale white solid product (1.6 g, yield 43%). MS (m/z): 277 (M+H).

1. temperatureThe resulting mixture was heated
2. temperatureto reflux for 4 days
3. customThe solvent was removed in vacuo
4. customethyl acetate, and the ethyl acetate layer was separated
5. concentrationconcentrated
6. customThe product was purified by silica gel column chromatography