反应详情

HBTU (296 mg, 0.78 mmol) was added to a solution of 1-(3,3-dimethyl-butyl)-piperidine-4-carboxylic acid from Example E15 (182 mg, 0.73 mmol) in DMF (5 ml) and DIEA (0.272 ml, 1.56 mmol). The mixture was stirred at room temperature for 2 h then 4-aminomethyl-N-(4-chloro-phenyl)-3,N-dimethyl-benzamide from Example E115.2 (150 mg, 0.52 mmol) was added. The mixture was stirred for 2 h at room temperature then diluted with EtOAc, 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 (209 mg, 83%).

1. stirringThe mixture was stirred for 2 h at 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