反应详情

温度

95 °C

6-benzyl-4-chloro-5,6,7,8-tetrahydro-pyrido[4,3-d]pyrimidin-2-ylamine (1.92 g., 7 mmoles) and 2-chlorophenylboronic acid (1.09 g., 7 mmoles) were mixed and stirred in a mixture of acetonitrile and water (50:50, 32 mls); anhydrous potassium carbonate (1.93 g., 14 mmoles) was then added to the stirred reaction mixture under nitrogen. Pd(PPh3)4 (0.2 g.) was then added to the reaction mixture which was stirred and heated at 95° C. for 3 hours also under nitrogen. The reaction mixture was then allowed to cool to room temperature and a beige solid formed. This suspension was quenched with water (150 mls) and the solid filtered and washed with water (100 mls) dried in a vacuum desiccator. The product was then eluted through a ‘silica plug’ in ethyl acetate, after evaporation the solid was slurried in ether to give, after filtering and drying a white solid (1.5 g., 61.2% yield). LC-MS (retention 2.65 mins, mass 351 M+H).

1. temperatureto cool to room temperature
2. customa beige solid formed
3. customThis suspension was quenched with water (150 mls)
4. filtrationthe solid filtered
5. washwashed with water (100 mls)
6. customdried in a vacuum desiccator
7. washThe product was then eluted through a ‘silica plug’ in ethyl acetate
8. customafter evaporation the solid
9. customto give
10. filtrationafter filtering
11. customdrying a white solid (1.5 g., 61.2% yield)
12. customLC-MS (retention 2.65 mins, mass 351 M+H)