반응 #1184828

반응 방정식

8-chloro-7-(2-propen-1-yl)-3-(4,4,4-trifluorobutyl)-3,7-dihydro-1H-purine-2,6-dione

caesium carbonate

3-bromo-1-propanol

→

title compound

수율 75.0%

8-Chloro-1-(3-hydroxypropyl)-7-(2-propen-1-yl)-3-(4,4,4-trifluorobutyl)-3,7-dihydro-1H-purine-2,6-dione

수율 75.0%

용매

DMF

반응 조건

후처리

1. 1
   온도cooled
2. 2
   기타evaporated
3. 3
   기타The residue was partitioned between EtOAc (50 ml) and water (50 ml)
4. 4
   건조The organic phase was dried (MgSO4)
5. 5
   여과filtered
6. 6
   기타evaporated
7. 7
   기타The product was purified by flash chromatography
8. 8
   세척a gradient elution from cyclohexane to EtOAc
9. 9
   기타evaporated

실험 절차

A solution of 8-chloro-7-(2-propen-1-yl)-3-(4,4,4-trifluorobutyl)-3,7-dihydro-1H-purine-2,6-dione (1.0 g, 3.0 mmol) in DMF (15 ml) was treated with caesium carbonate (1.16 g, 3.6 mmol) and 3-bromo-1-propanol (0.3 ml, 3.3 mmol). The mixture was heated at 60° C. for 4 h and then cooled and evaporated. The residue was partitioned between EtOAc (50 ml) and water (50 ml). The organic phase was dried (MgSO4), filtered and evaporated. The product was purified by flash chromatography using a gradient elution from cyclohexane to EtOAc. Product-containing fractions were combined and evaporated to give the title compound as a colourless oil (0.82 g, 75%).

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