反应详情

CDl (0.98 g, 6.1 mmol) was added to a solution of 5-(3-butyl-8-chloro-2,6-dioxo-2,3,6,7-tetrahydro-1H-purin-1-yl)pentanoic acid (1.89 g, 5.5 mmol) in DMF (15 ml) and stirred under nitrogen for 1.5 h. Benzamidoxime (0.91 g, 6.1 mmol) was added and the mixture stirred at 110° C. overnight. The reaction mixture was partitioned between EtOAc and 2M HCl. The organic layer was separated, washed with brine, dried (MgSO4) and evaporated. The crude product was crystallised from methanol and then further purified using the Companion™ system and a gradient elution from cyclohexane to EtOAc. Product containing fractions were combined and evaporated to give the title compound as a white solid (850 mg).

1. stirringthe mixture stirred at 110° C. overnight
2. customThe reaction mixture was partitioned between EtOAc and 2M HCl
3. customThe organic layer was separated
4. washwashed with brine
5. dry with materialdried (MgSO4)
6. customevaporated
7. customThe crude product was crystallised from methanol
8. customfurther purified
9. washa gradient elution from cyclohexane to EtOAc
10. additionProduct containing fractions
11. customevaporated