反应详情

A solution of 3-(4-{[6-(benzyl{(2R)-2-[4-(benzyloxy)-3-(formylamino)phenyl]-2-hydroxyethyl}amino)hexyl]oxy}but-1-ynyl)benzenesulfonamide (320 mg) in ethanol (15 ml) was hydrogenated in the presence of 10% palladium on carbon (50 mg) and palladium hydroxide on carbon (100 mg) at 100 p.s.i for 18 h. The catalyst was filtered off onto celite and the filtrate was evaporated to dryness. The residual oil was purified by chromatography on Biotage (8 g) cartridge eluting with dichloromethane/ethanol/0.88 ammonia (25:8:1). The residual oil (118 mg) was dissolved in methanol (20 ml) and treated with fumaric acid (0.5 equivalent) and evaporated to give the title compound (80 mg). LCMS RT=2.39 min, ES+ve 508 (MH)+.

1. filtrationThe catalyst was filtered off onto celite
2. customthe filtrate was evaporated to dryness
3. customThe residual oil was purified by chromatography on Biotage (8 g) cartridge
4. washeluting with dichloromethane/ethanol/0.88 ammonia (25:8:1)
5. dissolutionThe residual oil (118 mg) was dissolved in methanol (20 ml)
6. customevaporated