反应详情

To a round bottom flask add (2-{6-benzyloxy-1-[4-(2-piperidin-1-yl-ethoxy)-benzoyl]-naphthalen-2-yl}-5-fluoro-phenyl)-carbamic acid tert-butyl ester (0.075 g, 0.11 mmol), ammonium formate (0.056 g, 0.89 mmol), methanol (5 mL) and a slurry of 10% Pd/C (0.012 g, ˜15% by weight) and ethanol (2 mL). Heat the mixture, with stirring, at reflux for 30 minutes. Cool the reaction to ambient temperature and filter it through a pad of Celite, then rinse the Celite with hot methanol. Evaporate the filtrate in vacuo and purify the resulting residue by radial chromatography over silica (4-9% MeOH gradient in CH2Cl2) to provide the product 61 mg (94%): mass spectrum (ion spray) m/z=585 (M+H).

1. temperatureHeat the mixture
2. temperatureat reflux for 30 minutes
3. temperatureCool
4. customthe reaction to ambient temperature
5. filtrationfilter it through a pad of Celite
6. washrinse the Celite with hot methanol
7. customEvaporate the filtrate in vacuo
8. custompurify the resulting residue by radial chromatography over silica (4-9% MeOH gradient in CH2Cl2)