反应详情

温度

2.5 °C

N-Bromosuccinimide (1.182 g, 6.64 mmol) was added portionwise to a solution of 2-{[(1S)-1-methylpropyl]oxy}-9-(tetrahydro-2H-pyran-2-yl)-9H-purin-6-amine (1.935 g, 6.64 mmol) in chloroform (50 ml) at 0-5° C. The resulting green solution was stirred at 0-5° C. for 1 hour during which time it turned red and the mixture was then allowed to warm to room temperature and stirred overnight. The resulting green solution was washed with water (2×20 ml), separated using a hydrophobic frit and concentrated. The residue was dissolved in dichloromethane and purified by silica gel chromatography (100 g cartridge) using a Flashmaster II apparatus and a 0-100% ethyl acetate-cyclohexane gradient over 60 mins. The appropriate fractions were combined and evaporated in vacuo to give the title compound as a yellow foam (1.79 g).

1. temperatureto warm to room temperature
2. stirringstirred overnight
3. washThe resulting green solution was washed with water (2×20 ml)
4. customseparated
5. concentrationconcentrated
6. dissolutionThe residue was dissolved in dichloromethane
7. custompurified by silica gel chromatography (100 g cartridge)
8. waita 0-100% ethyl acetate-cyclohexane gradient over 60 mins
9. customevaporated in vacuo