反应详情

温度

-78 °C

9.4 mL 2.5 mol/L butyllithium solution in THF was added dropwise to 11.8 g 2-(4,5-dibromo-2-phenyl-imidazol-1-yl)-1-(4-pyrimidin-2-yl-piperazin-1-yl)-ethanone in 150 mL THF at −78° C. under argon. The reaction mixture was stirred 2 h at −78° C. followed by careful and dropwise addition of water to the mixture. The resulting mixture was stirred 30 min at −78° C. and then again water was added at 0° C. The mixture was extracted with ethyl acetate. The organic layer was dried and evaporated. The residue was purified chromatoraphie on silica (petrolether 1/ethylacetate 1). Diisopropylether was added to the residue and the precipitate was filtered and dried to give 1.7 g desired product. Rt: 0.94 (method B), ESI+: 427

1. stirringThe resulting mixture was stirred 30 min at −78° C.
2. extractionThe mixture was extracted with ethyl acetate
3. customThe organic layer was dried
4. customevaporated
5. customThe residue was purified chromatoraphie on silica (petrolether 1/ethylacetate 1)
6. additionDiisopropylether was added to the residue
7. filtrationthe precipitate was filtered
8. customdried