反应详情

(1R*,2R*,5S*,6R*)-8-Benzyl-2-{(1R*)-1-[3,5-bis(trifluoromethyl)phenyl]-2-phenylmethoxyethoxy}-6-cyano-1-phenyl-8-azabicyclo[3.2.1]octane (Example 157; 0.7105 g, 1.07 mmol), sodium azide (0.2087 g, 3.21 mmol) and ammonium chloride (0.172 g, 3.21 mmol) in dimethylformamide (10 ml) were heated at 120° C. for 18 hours. A further 3.0 eq of sodium azide and 3.0 eq of triethylamine hydrochloride were added and the mixture heated for a further 18 hours. The mixture was diluted with ethyl acetate and washed with water. The organics were collected, dried (MgSO4) and concentrated in vacuo. The residue was purified by flash column chromatography, eluting with 5% methanol/dichloromethane to give the title compound (400 mg, 53%).

1. temperaturethe mixture heated for a further 18 hours
2. washwashed with water
3. customThe organics were collected
4. dry with materialdried (MgSO4)
5. concentrationconcentrated in vacuo
6. customThe residue was purified by flash column chromatography
7. washeluting with 5% methanol/dichloromethane