反应详情

A solution of 4-iodo-2-benzofuran-1,3-dione (0.55 g, 2.01 mmol) and urea (0.24 g, 3.99 mmol) in xylene (5 mL) was heated to reflux overnight. After cooling, the solvent was removed in vacuo and the residue partitioned between water and ethyl acetate. The aqueous phase was extracted with ethyl acetate and the combined organic layers washed with brine, dried over MgSO4 and concentrated in vacuo while loading onto silica. Dry flash column chromatography using 5–10% ethyl acetate/isohexane gave 4-iodo-1H-isoindole-1,3 (2H)-dione as a pale yellow solid (330 mg, 60%).

1. temperatureto reflux overnight
2. temperatureAfter cooling
3. customthe solvent was removed in vacuo
4. customthe residue partitioned between water and ethyl acetate
5. extractionThe aqueous phase was extracted with ethyl acetate
6. washthe combined organic layers washed with brine
7. dry with materialdried over MgSO4
8. concentrationconcentrated in vacuo
9. customDry flash column chromatography