反应详情

A mixture of 3-[4-(2,3,4,5-tetrahydro-benzo[b]azepine-1-carbonyl)-phenyl]-propionic acid from Example E65.4 (57 mg, 0.18 mmol) and thionyl chloride (0.2 ml, 2.74 mmol) in dichloromethane (6 ml) was heated at reflux for 2 h then volatiles were removed in vacuo. The residue was dissolved in dichloromethane (8 ml) then benzylamine (0.022 ml, 0.20 mmol) and triethylamine (0.05 ml, 0.36 mmol) were added. The mixture was stirred for 3 h at room temperature then concentrated in vacuo. The residue was purified by flash chromatography on silica gel (eluant; 30% pet. ether:70% EtOAc) to give a white fluffy solid identified as the title compound (36.5 mg, 50%).

1. temperaturewas heated
2. temperatureat reflux for 2 h
3. customwere removed in vacuo
4. dissolutionThe residue was dissolved in dichloromethane (8 ml)
5. concentrationthen concentrated in vacuo
6. customThe residue was purified by flash chromatography on silica gel (eluant; 30% pet. ether:70% EtOAc)
7. customto give a white fluffy solid