反应详情

温度

0 °C

2-(Butyloxy)-9-(tetrahydro-2H-pyran-2-yl)-9H-purin-6-amine (9.45 g) was dissolved in chloroform (50 ml) and cooled to 0° C. (ice-bath). To this solution was added portion wise N-bromosuccinimide (6.07 g) keeping the temperature below 3° C. This gave a dark green solution, stirred at 2.5° C. for 30 mins. before allowing to warm to room temperature and then stirring for 6 hours. The reaction mixture was then washed with water (100 ml, twice). Organic phase was dried/separated using a hydrophobic frit and evaporated to give a dark brown gum which was purified by silica chromatography (120 g) (ISCO) using a gradient elution of 0-50% ethyl acetate: cyclohexane to afford the title compound as a pale yellow solid (8.37 g).

1. customthe temperature below 3° C
2. customThis gave a dark green solution
3. temperatureto warm to room temperature
4. stirringstirring for 6 hours
5. washThe reaction mixture was then washed with water (100 ml
6. customOrganic phase was dried/separated
7. customevaporated
8. customto give a dark brown gum which
9. customwas purified by silica chromatography (120 g) (ISCO)
10. washa gradient elution of 0-50% ethyl acetate