反应详情

DIEA (0.135 ml, 0.78 mmol) and butyryl chloride (0.027 ml, 0.27 mmol) were added to a solution of (4-aminomethyl-3-fluoro-phenyl)-(6-chloro-3-methyl-4,10-dihydro-3H-2,3,4,9-tetraaza-benzo[f]azulen-9-yl)-methanone hydro-chloride from Example E102.2 (110 mg, 0.26 mmol) in di-chloromethane (3 ml) at room temperature. The mixture was stirred for 1 h, washed with saturated NaHCO3 then brine, dried and concentrated in vacuo. The residue was purified by preparative HPLC (eluant; 0.5% 35% ammonia:9.5% methanol:90% dichloromethane) to give a white powder identified as the title compound (77 mg, 65%).

1. customat room temperature
2. washwashed with saturated NaHCO3
3. dry with materialbrine, dried
4. concentrationconcentrated in vacuo
5. customThe residue was purified by preparative HPLC (eluant; 0.5% 35% ammonia:9.5% methanol:90% dichloromethane)
6. customto give a white powder