反应详情

温度

100 °C

A mixture of ethyl 3-{[(benzyloxy)carbonyl]amino}-7-bromoquinoline-2-carboxylate (300 mg, 0.7 mmol), morpholine (120 mg, 1.4 mmol), Pd(OAc)2 (20 mg), dicyclohexyl(2′,6′-diisopropoxybiphenyl-2-yl)phosphine (49 mg, 0.10 mmol), and K3PO4 (580 mg, 2.8 mmol) in tert-butanol (10 mL) in a sealed vial was purged with nitrogen then heated at 100° C. for 1 h. The solution was allowed to cool then and diluted with EtOAc, and the mixture was filtered through diatomaceous earth. The filtrate was concentrated under reduced pressure, and the resulting residue was purified by flash chromatography on 40 g of silica gel, eluting with 0-100% EtOAc in hexanes, to give the sub-title compound (0.3 g, 20%). LCMS (ESI) calc. for C24H26N3O5 [M+H]+: m/z=436.2. found: 436.1.

1. customvial was purged with nitrogen
2. temperatureto cool
3. additiondiluted with EtOAc
4. filtrationthe mixture was filtered through diatomaceous earth
5. concentrationThe filtrate was concentrated under reduced pressure
6. customthe resulting residue was purified by flash chromatography on 40 g of silica gel
7. washeluting with 0-100% EtOAc in hexanes