反应详情

温度

0 °C

To a suspension of (S)-1-(2-bromo-6-methyl-4-nitrophenyl)ethane-1,2-diol (65D) (6.96 g, 25.22 mmol) in DCM (100 ml), was added pyridine (5 mL) at 0° C. To the solution was added pivaloyl chloride (PivCl) slowly at 0° C. The reaction mixture was stirred at 0° C. for 5 min, then raised to rt, stirred at rt for 5 h. The reaction mixture was washed by sat. NaHCO3, extracted by DCM, dry over MgSO4, filtered, purified by silica gel column, eluting by 0-40% EtOAc in Hexanes to give 9.13 g of 65E. The product taken on without full characterization.

1. temperatureraised to rt
2. stirringstirred at rt for 5 h
3. washThe reaction mixture was washed by sat. NaHCO3
4. extractionextracted by DCM
5. dry with materialdry over MgSO4
6. filtrationfiltered
7. custompurified by silica gel column
8. washeluting by 0-40% EtOAc in Hexanes