反应详情

A mixture of Intermediate 9 (435 mg) and Sodium hydroxide, 2M aq (2.3 mL) in Ethanol (6 mL) was stirred at RT for 5 mins and then at 80° C. for 3 hr. The solvent was concentrated under vacuum, the residue suspended in acetic acid (6.00 mL) and heated at 120° C. for 2 hr. The solvent was removed under vacuum and the residue was purified by reverse phase chromatography using acetonitrile water with an ammonium carbonate modifier. The desired fractions were combined and concentrated under vacuum to give a white solid (210 mg). LC/MS MH+ 395, Rt 2.10 min (5 minute run).

1. waitat 80° C. for 3 hr
2. concentrationThe solvent was concentrated under vacuum
3. temperatureheated at 120° C. for 2 hr
4. customThe solvent was removed under vacuum
5. customthe residue was purified by reverse phase chromatography
6. concentrationconcentrated under vacuum