反应详情

温度

0 °C

47 mg of sodium hydride were added portionwise to a solution of 300 mg of 3-(4,5-diphenyl-1H-imidazol-2-yl)-propionic acid methyl ester in 2 mL of anh. DMF at 0° C. The mixture was stirred for 1 h at 0° C. then 179 mg of SEM-Cl were added dropwise at 0° C. The reaction mixture was allowed to warm up to rt, stirred for 1 h then poured into water and extracted with Et2O. The organic phase was washed with water/brine, dried over anh. Na2SO4 and concentrated in vacuo. The resulting crude material was purified by CC using heptane/EtOAc from 88/12 to 0/100 as eluant to yield 308 mg of 3-[4,5-diphenyl-1-(2-trimethylsilanyl-ethoxymethyl)-1H-imidazol-2-yl]-propionic acid methyl ester as a yellowish oil.

1. temperatureto warm up to rt
2. stirringstirred for 1 h
3. extractionextracted with Et2O
4. washThe organic phase was washed with water/brine
5. dry with materialdried over anh. Na2SO4
6. concentrationconcentrated in vacuo
7. customThe resulting crude material was purified by CC