反应详情

3-{4-[6-(1-Hydroxymethyl-propylamino)-2-oxo-3-propyl-3,7-dihydro-2H-purin-8-yl]-bicyclo[2.2.2]oct-1-yl}-propionic acid methyl ester (30 mg) was dissolved in 1 mL of SOCl2 and stirred under reflux for 15 min. The reaction mixture was then cooled to rt and concentrated under reduced pressure. The resulting residue was dissolved in a solution containing 1 mL of water, 0.5 mL of MeOH, and 0.1 mL of 10% aq. NaOH. The reaction mixture was stirred at rt for 30 min. It was then acidified to pH 2 with dilute 1 N HCl and concentrated. The resulting crude product was purified by preparative HPLC to afford the titled compound.

1. temperatureunder reflux for 15 min
2. concentrationconcentrated under reduced pressure
3. dissolutionThe resulting residue was dissolved in a solution
4. additioncontaining 1 mL of water, 0.5 mL of MeOH, and 0.1 mL of 10% aq. NaOH
5. stirringThe reaction mixture was stirred at rt for 30 min
6. additionwith dilute 1 N HCl
7. concentrationconcentrated
8. customThe resulting crude product was purified by preparative HPLC