反应详情

温度

-40 °C

Into a flask containing methyl 2-bromo-1-((2-(trimethylsilyl)ethoxy)methyl)-1H-imidazole-4-carboxylate (5 g, 14.9 mmol) in THF (20 ml), 2 M solution of i-PrMgCl in THF (22.4 ml, 44.9 mmol) was added at −40° C. under nitrogen atmosphere. The resulting mixture was allowed to stir for 10 min at −40° C. and cooled to −78° C. The reaction mixture was treated with DMF (7.29 ml, 89.8 mmol) and slowly warmed to RT. The mixture was stirred for 1 h at RT and quenched with saturated aqueous solution of NaHCO3. The crude was extracted with EtOAc. The organic layer was concentrated under reduced pressure. Yield 3 g. LC-MS: [M+1]=285.15.

1. additionwas added at −40° C. under nitrogen atmosphere
2. temperaturecooled to −78° C
3. temperatureslowly warmed to RT
4. stirringThe mixture was stirred for 1 h at RT
5. customquenched with saturated aqueous solution of NaHCO3
6. extractionThe crude was extracted with EtOAc
7. concentrationThe organic layer was concentrated under reduced pressure