反应详情

A solution of Example 316 (2.13 g, 11.6 mmol) and N-iodosuccinimide (3.13 g, 13.9 mmol) in N,N-dimethylformamide (45 mL) was heated to about 80° C. for about 5 hours. The reaction mixture was cooled to room temperature and was concentrated in high vacuum. The residue was partitioned between water and ethyl acetate, the layers were separated and the aqueous layer was extracted with ethyl acetate. The combined organic extracts were dried (MgSO4), filtered and concentrated under vacuum. The residue was purified by flash chromatography on silica gel using hexane/ethyl acetate (2:1) as eluent to provide the desired product. MS (ESI): m/z 309 (M−H)−.

1. concentrationwas concentrated in high vacuum
2. customThe residue was partitioned between water and ethyl acetate
3. customthe layers were separated
4. extractionthe aqueous layer was extracted with ethyl acetate
5. dry with materialThe combined organic extracts were dried (MgSO4)
6. filtrationfiltered
7. concentrationconcentrated under vacuum
8. customThe residue was purified by flash chromatography on silica gel