反应详情

A mixture of 2,4,5-tribromo-1-((2-(trimethylsilyl)ethoxy)methyl)-1H-imidazole (653 mg, 1.5 mmol) and piperazine (1.03 g, 12.0 mmol) under Ar was irradiated at 130° C. for 15 min in a microwave reactor. The reaction mixture was partitioned between DCM and water (100 mL, 1/1). The layers were separated and the aqueous layer was extracted with DCM (2×50 mL). The combined organic layers were dried (Na2SO4), filtered and concentrated in vacuo. The resulting was purified by flash chromatography (SiO2, 100:0-90:10 DCM-MeOH) to provide 186 mg of 1-(4,5-dibromo-1-((2-(trimethylsilyl)ethoxy)methyl)-1H-imidazol-2-yl)piperazine as a colorless oil:

1. customwas irradiated at 130° C. for 15 min in a microwave reactor
2. customThe reaction mixture was partitioned between DCM and water (100 mL, 1/1)
3. customThe layers were separated
4. extractionthe aqueous layer was extracted with DCM (2×50 mL)
5. dry with materialThe combined organic layers were dried (Na2SO4)
6. filtrationfiltered
7. concentrationconcentrated in vacuo
8. customThe resulting was purified by flash chromatography (SiO2, 100:0-90:10 DCM-MeOH)