反应详情

温度

60 °C

A solution of 8-chloro-7-(2-propen-1-yl)-3-propyl-3,7-dihydro-1H-purine-2,6-dione (3.0 g, 11.1 mmol) in DMF (20 ml) was treated with caesium carbonate (3.7 g, 11.4 mmol) and 3-bromo-1-propanol (1.6 g, 11.5 mmol). The mixture was heated at 60° C. for 4 h and then cooled and evaporated. The residue was partitioned between EtOAc (60 ml) and saturated aqueous sodium bicarbonate (50 ml). The aqueous phase was extracted with EtOAc (60 ml), the combined organic phases were dried (MgSO4), filtered and evaporated. The product was purified using the Companion™ system and a gradient elution from cyclohexane to EtOAc. Product containing fractions were combined and evaporated to give the title compound as a colourless oil (2.6 g).

1. temperaturecooled
2. customevaporated
3. customThe residue was partitioned between EtOAc (60 ml) and saturated aqueous sodium bicarbonate (50 ml)
4. extractionThe aqueous phase was extracted with EtOAc (60 ml)
5. dry with materialthe combined organic phases were dried (MgSO4)
6. filtrationfiltered
7. customevaporated
8. customThe product was purified
9. washa gradient elution from cyclohexane to EtOAc
10. additionProduct containing fractions
11. customevaporated