反应详情

温度

0 °C

The reaction mixture of 1-bromo-3-methyl-5-nitro-2-vinylbenzene (65C) (12.3 g, 50.83 mmol), AD-mix a (71 g), MeSO2NH2 (4.8 g, 50.8 mmol) in t-butyl alcohol/H2O (1:1) (200 ml) was stirred at 0° C. for 3 days. Na2SO3 (˜6 g) was added to quench the reaction, stirred at rt for 40 min. The reaction mixture was washed by water, extracted by EtOAc, dry over MgSO4, filtered, concentrated down and purified by silica gel column, eluting by 0-100% EtOAc in Hexanes to give 6.96 g of 65D and recovered 2.3 g of 65C.

1. customto quench
2. customthe reaction
3. stirringstirred at rt for 40 min
4. washThe reaction mixture was washed by water
5. extractionextracted by EtOAc
6. dry with materialdry over MgSO4
7. filtrationfiltered
8. concentrationconcentrated down
9. custompurified by silica gel column
10. washeluting by 0-100% EtOAc in Hexanes