反应详情

1-methyl-3-pentyl-7-(2-propen-1-yl)-3,7-dihydro-1H-purine-2,6-dione (0.45 g, 1.63 mmol), phenylsilane (0.25 ml, 2.03 mmol) and tetrakis(triphenylphosphine)palladium(0) (0.35 g, 0.3 mmol) was dissolved in DCM (10 ml) containing acetic acid (6 ml). The air in the flask was replaced by nitrogen by evacuating the flask then filling with nitrogen (×3) and the reaction mixture heated to 45 C for 4 h. The solution was allowed to cool diluted with DCM then washed with water then saturated sodium bicarbonate solution. The organics were isolated, dried and concentrated to yield crude product. Purification by SPE (silica) eluting with ether provided the product, 0.06 g, 16%. m/z 237 [MH+].

1. customby evacuating the flask
2. temperaturethe reaction mixture heated to 45 C for 4 h
3. temperatureto cool
4. additiondiluted with DCM
5. washthen washed with water
6. customThe organics were isolated
7. customdried
8. concentrationconcentrated
9. customto yield crude product
10. customPurification by SPE (silica)
11. washeluting with ether
12. customprovided the product, 0.06 g, 16%