反应详情

A stirred mixture of 2-(2-ethoxybenzamido)-3-methoxybenzamide (2.6 g, 0.0083 mol), anhydrous potassium carbonate (2.33 g, 0.017 mol), hydrogen peroxide (30%, 4 ml), ethanol (40 ml) and water (80 ml) was heated under reflux for 1 hour. The mixture was allowed to cool and poured into a mixture of water (200 ml) and dichloromethane (100 ml), then the aqueous phase separated, acidified to pH 4 by the addition of 2N hydrochloric acid and extracted with dichloromethane (2×100 ml). The organic solutions were combined, dried (MgSO4) and evaporated under vacuum to give the title compound, which crystallized from ethyl acetate as a colorless solid (2.8 g, 83%), m.p. 198°-199° C. Found: C,68.88; H,5.50; N,9.30. C17H16N2O3 requires C,68.91; H,5.44; N,9.45%.

1. temperaturewas heated
2. temperatureunder reflux for 1 hour
3. temperatureto cool
4. customthe aqueous phase separated
5. additionacidified to pH 4 by the addition of 2N hydrochloric acid
6. extractionextracted with dichloromethane (2×100 ml)
7. dry with materialdried (MgSO4)
8. customevaporated under vacuum