反应详情

温度

80 °C

3-butyl-8-chloro-7-(2-propen-1-yl)-3,7-dihydro-1H-purine-2,6-dione (2.0 g, 0.0072 mol) in dry MeCN (20 ml) was added Cs2CO3 (4.68 g, 0.0144 mol) followed by bromobutyronitrile (1.38 g, 0.0094 mol). The mixture was heated at 80° C. for 18 h and then allowed to cool. The reaction mixture was evaporated and the crude product partitioned between EtOAc and HCl (2N). The organic phase was separated and washed with brine, dried (MgSO4) and evaporated to give the crude product. This was purified by silica SPE (50 g), eluting with cyclohexane:ethylacetate (2:1 to 1:1) to afford the title compound as a clear oil (2.1 g, 85%).

1. temperatureto cool
2. customThe reaction mixture was evaporated
3. customthe crude product partitioned between EtOAc and HCl (2N)
4. customThe organic phase was separated
5. washwashed with brine
6. dry with materialdried (MgSO4)
7. customevaporated
8. customto give the crude product
9. customThis was purified by silica SPE (50 g)
10. washeluting with cyclohexane:ethylacetate (2:1 to 1:1)