反应详情

A mixture of 5-bromo-2-chloropyrimidine (5.17 mmol) and 1,1-dimethylethyl 1-piperazinecarboxylate (11.4 mmol) in 1,4-dioxane (10 ml) was heated at reflux for 2 hours. After cooling to room temperature, the reaction mixture was diluted with water (100 ml) and ethyl acetate (100 ml). Separation of the organic layer, drying (MgSO4), filtration and concentration in vacuo provided a residue which was purified by silica gel chromatography (40 g silica gel, CHCl3/EtOAc) to give the title compound as a white solid (58%). ESMS [M+H-Boc]+: 245.0/243.0.

1. temperaturewas heated
2. temperatureat reflux for 2 hours
3. customSeparation of the organic layer
4. customdrying
5. filtration(MgSO4), filtration and concentration in vacuo
6. customprovided a residue which
7. customwas purified by silica gel chromatography (40 g silica gel, CHCl3/EtOAc)