反应详情

Combine N-Boc-5-hydroxy-2-aminoindane (2.50 g, 10.0 mmol), 6-chloronicotinamide (1.49 g, 9.55 mmol K2CO3 (1.90 g, 14.3 mmol), DMA (25 ml) and toluene (20 ml) in a round bottom flask, equipped with Dean-Stark trap, condenser, and nitrogen inlet. Reflux the suspension for two hours before cooling to ambient temperature. Remove the solids via filtration, wash solids with EtOAc, and concentrate the filtrate/wash on a rotary evaporator. Dissolve the remaining oil in EtOAc, wash with water (2×) and brine, dry (MgSO4) and concentrate. Purify the material on silica gel (20% THF/DCM) to give [5-(5-carbamoyl-pyridin-2-yloxy)-indan-2-yl]carbamic acid tert-butyl ester (870 mg) as a light yellow solid.

1. temperatureReflux the suspension for two hours
2. customRemove the solids
3. filtrationvia filtration
4. washwash solids with EtOAc
5. concentrationconcentrate the
6. washfiltrate/wash on a rotary evaporator
7. dissolutionDissolve the remaining oil in EtOAc
8. washwash with water (2×) and brine
9. dry with materialdry (MgSO4)
10. concentrationconcentrate
11. customPurify the material on silica gel (20% THF/DCM)