反应详情

WSCD (58 mg, 0.30 mmol) and DMAP (20 mg, 0.15 mmol) were added to a solution of 3-methyl-3,4,9,10-tetrahydro-2,3,4,9-tetraaza-benzo[f]azulene from Example E11 (37 mg, 0.20 mmol) and 4-{2-[4-(3,3-dimethyl-butyl)-piperazin-1-yl]-ethoxy}-3-methyl-benzoic acid from Example E40 (53 mg, 0.15 mmol) in dichloromethane (5 ml) and triethylamine (to pH9). The mixture was heated at re-flux for 2 days then concentrated in vacuo. The residue was dissolved in EtOAC, washed with saturated NaHCO3 then brine, dried and concentrated in vacuo. The residue was purified by flash chromatography on silica gel (eluant; 10% methanol:90% chloroform) to give an off-white solid identified as the title compound (3.5 mg, 4%).

1. temperatureThe mixture was heated at re-flux for 2 days
2. concentrationthen concentrated in vacuo
3. dissolutionThe residue was dissolved in EtOAC
4. washwashed with saturated NaHCO3
5. dry with materialbrine, dried
6. concentrationconcentrated in vacuo
7. customThe residue was purified by flash chromatography on silica gel (eluant; 10% methanol:90% chloroform)
8. customto give an off-white solid