反应详情

A mixture of 1-(7,8-dihydroxyoctyl)-3,7-dimethylxanthine, prepared as described above, (2.11 g, 6 mmol) was stirred with a 30% solution of hydrogen bromide in acetic acid (3.58 mL, 18 mmol) for 90 minutes. The mixture was then added to a flask containing aqueous sodium bicarbonate solution (4 g in 50 mL) and dichloromethane (30 mL). After 10 minutes of vigorous stirring the layers were separated and the aqueous portion was washed with dichloromethane (2×50 mL). The combined organic portions were dried over sodium sulfate and the solvent was evaporated under vacuum, yielding 2.51 g (94%) 1-(7-acetoxy-8-bromooctyl)-3,7-dimethylxanthine (inventive compound no. 1514) as a yellow oil.

1. customprepared
2. additionThe mixture was then added to a flask
3. customwere separated
4. washthe aqueous portion was washed with dichloromethane (2×50 mL)
5. dry with materialThe combined organic portions were dried over sodium sulfate
6. customthe solvent was evaporated under vacuum