反应详情

A mixture of 3,4-difluoro-N,2-dihydroxybenzamide (Intermediate 527, 7.91 g, 41.8 mmol) and carbonyl diimidazole (13.6 g, 83.7 mmol) in THF (200 ml) was heated at reflux for 90 min. The mixture was partitioned between EtOAC and water and acidified with conc. HCl. The solution was extracted 3 times with EtOAc, each extract being washed with water and brine. Drying (MgSO4) of the combined extracts and removal of solvent gave 6.88 g of product as an off-white solid.

1. temperaturewas heated
2. temperatureat reflux for 90 min
3. customThe mixture was partitioned between EtOAC and water
4. extractionThe solution was extracted 3 times with EtOAc
5. washeach extract being washed with water and brine
6. customDrying
7. custom(MgSO4) of the combined extracts and removal of solvent