反应详情

3-[4-(2,6-Dioxo-3-propyl-2,3,6,7-tetrahydro-1H-purin-8-yl)-bicyclo[2.2.2]oct-1-yl]-propionic acid methyl ester (250 mg, 0.64 mmol) was dissolved in 8 mL of pyridine. P4S10 (430 mg, 1.5 eq) was added and the reaction mixture was stirred under reflux for 3 h. It was then cooled to rt and quenched with 3 mL of H2O and then with enough 6 N HCl to bring the pH to 3. The resulting reaction mixture was extracted with CHCl3. The organic layer was dried (Na2SO4) and concentrated under reduced pressure. The crude residue was purified by preparative HPLC to afford 100 mg of the desired product.

1. temperatureunder reflux for 3 h
2. customquenched with 3 mL of H2O
3. customThe resulting reaction mixture
4. extractionwas extracted with CHCl3
5. dry with materialThe organic layer was dried (Na2SO4)
6. concentrationconcentrated under reduced pressure
7. customThe crude residue was purified by preparative HPLC