反应详情

温度

150 °C

5,6,7,8-Tetrahydro-3H-pyrido[3,4-d]pyrimidin-4-one (1.5 g, 10 mmol) was dissolved in a mixture of dioxane-dimethylacetamide (2 ml, 3:1) and 2,3-dichloropyridine was added (1.5 g, 10 mmol), followed by DIEA (1.7 ml; 10 mmol). The mixture was heated at 150° C. for 2 hours in a microwave (Personal Chemistry, Smith Creator). The solvents were evaporated and the residue was dissolved in a 3:1 mixture of chloroform-isopropanol and washed with water. The organic layer washed with brine, dried over soldium sulphate, filtered and evaporated to give a yellow solid (3 g). The crude material was used for the subsequent step.

1. additionwas added (1.5 g, 10 mmol)
2. customThe solvents were evaporated
3. dissolutionthe residue was dissolved in a 3:1 mixture of chloroform-isopropanol
4. washwashed with water
5. washThe organic layer washed with brine
6. customdried
7. filtrationfiltered
8. customevaporated