反应详情

DIEA (0.30 ml, 1.7 mmol) and 1,1′-carbonyldiimidazole (39 mg, 0.24 mmol) were added to a solution of (4-aminomethyl-cyclohexyl)-(3,6-dimethyl-4,10-dihydro-3H-2,3,4,9-tetraaza-benzo[f]azulen-9-yl)-methanone hydro-chloride (Compound number 149) (78 mg, 0.20 mmol) in DMF (4.0 ml) and the mixture was stirred at room temperature for 2 h. 1-(3,3-Dimethyl-butyl)-piperazine dihydrochloride from Example E4 (56 mg, 0.23 mmol) was added and the mixture was stirred at room temperature for 18 h. The mixture was diluted with EtOAc, washed with brine, dried and concentrated in vacuo. The residue was purified by preparative HPLC (eluant; 10% methanol:90% di-chloromethane) to give a white solid identified as the title compound (32 mg, 29%).

1. stirringthe mixture was stirred at room temperature for 18 h
2. washwashed with brine
3. customdried
4. concentrationconcentrated in vacuo
5. customThe residue was purified by preparative HPLC (eluant; 10% methanol:90% di-chloromethane)
6. customto give a white solid