反应详情

N-Chlorosuccinimide (0.075 g) was added to a solution of 4-bromo-2-fluorobenzaldehyde oxime (Intermediate 50) (0.44 g) in DMF (1 ml) then heated for several minutes at 55°. The mixture was allowed to cool to <50° then more N-chlorosuccinimide (0.22 g) was added. After a few minutes the mixture was allowed to cool to room temp. then partitioned between water and ether. The layers were separated, the aqueous layer was re-extracted with ether (×2) and the combined organic extracts were washed with water and brine, dried (MgSO4) and concentrated under vacuum to give a white solid (0.46 g).

1. temperaturethen heated for several minutes at 55°
2. temperatureto cool to <50°
3. waitAfter a few minutes the mixture was allowed
4. temperatureto cool to room temp.
5. customthen partitioned between water and ether
6. customThe layers were separated
7. extractionthe aqueous layer was re-extracted with ether (×2)
8. washthe combined organic extracts were washed with water and brine
9. dry with materialdried (MgSO4)
10. concentrationconcentrated under vacuum