反应详情

温度

0 °C

To a solution of (S)-2-(2-bromo-6-methyl-4-nitrophenyl)-2-hydroxyethyl pivalate (65E) in t-butyl acetate at 0° C., was added HClO4 (perchloric acid) (5.45 ml) slowly, stirred at 0° C. for 5 min, then the reaction mixture was warmed up to rt and stirred for 3 hs. The mixture was diluted by EtOAc, washed by sat. NaHCO3, extracted by EtOAc, dry over MgSO4, filtered, concentrated down and purified by silica gel column, eluting by 0-100% EtOAc in Hexanes to give 65F (9 g, 85%).

1. temperaturethe reaction mixture was warmed up to rt
2. stirringstirred for 3 hs
3. washwashed by sat. NaHCO3
4. extractionextracted by EtOAc
5. dry with materialdry over MgSO4
6. filtrationfiltered
7. concentrationconcentrated down
8. custompurified by silica gel column
9. washeluting by 0-100% EtOAc in Hexanes