反应详情

To a solution of tert-butyl 4-(3-aminophenethyl)piperazine-1-carboxylate (7D, 1.0 eq) in THF (about 0.3 M 7D in THF) was added 5-isocyanato-2-methylpyridine (1.0 eq) dropwise. The resulting reaction mixture was stirred for 2 h. To the reaction mixture was added saturated aq. NaHCO3. The mixture was diluted with EtOAc, and the layers were separated. The organic layer was washed twice with saturated aq. NaHCO3 and once with brine. The organic layer was dried over Na2 SO4, filtered and concentrated in vacuo. Purification over silica gel using 5-12% MeOH/CH2Cl2 as the gradient eluant provided tert-butyl 4-(3-(3-(6-methylpyridin-3-yl)ureido)phenethyl)piperazine-1-carboxylate (7E, 63%).

1. customThe resulting reaction mixture
2. customthe layers were separated
3. washThe organic layer was washed twice with saturated aq. NaHCO3 and once with brine
4. customThe organic layer was dried over Na2 SO4
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. customPurification over silica gel using 5-12% MeOH/CH2Cl2 as the gradient eluant