反应详情

A stirred mixture of 3-carbamoyl-2-(2-ethoxybenzamido)benzamide (Preparation 18; 1 g, 0.003 mol) sodium hydroxide (0.61 g, 0.015 mol), water (30 ml) and ethanol (7 ml) was heated under reflux for 1 hour. The cool solution was washed with dichloromethane (3×30 ml), acidified to pH 1 with 2N hydrochloric acid and the resulting precipitate collected by filtration. The solid was suspended in saturated aqueous sodium carbonate solution (60 ml) and this suspension extracted with dichloromethane-methanol (98:2, 3×100 ml). The extracts were combined, dried (Na2SO4) and evaporated under vacuum, then the residue triturated with diethyl ether (50 ml) to give the title compound as a white solid (0.72 g, 78%), m.p. 252-254° C.

1. temperaturewas heated
2. temperatureunder reflux for 1 hour
3. washThe cool solution was washed with dichloromethane (3×30 ml)
4. filtrationthe resulting precipitate collected by filtration
5. extractionthis suspension extracted with dichloromethane-methanol (98:2, 3×100 ml)
6. dry with materialdried (Na2SO4)
7. customevaporated under vacuum
8. customthe residue triturated with diethyl ether (50 ml)