反应详情

温度

210 °C

A mixture of 3-(2-ethoxybenzoylamino)-4-n-propylpridine-2-carboxamide (Preparation 7; 1.52 g, 0.0046 mol) and anhydrous zinc chloride (1.88 g, 0.014 mol) was heated at 210° C. for 0.25 hour. The cool mixture was dissolved in methanol (20 ml) and this solution poured into an aqueous solution of disodium ethylenediamine tetraacetic acid (10.3 g in 200 ml water). The resulting mixture was basified with saturated aqueous sodium carbonate solution (20 ml), then extracted with dichloromethane (4×60 ml). The combined organic extracts were dried (MgSO4) and evaporated under vacuum, then the residue crystallised from ethyl acetate to give the title compound as a white solid (0.92 g, 65%), m.p. 134°-137° C. Found: C,69.69; H,6.27; N,13.54. C18H19N3O2 requires C,69.88; H,6.19; N,13.58%.

1. extractionextracted with dichloromethane (4×60 ml)
2. dry with materialThe combined organic extracts were dried (MgSO4)
3. customevaporated under vacuum
4. customthe residue crystallised from ethyl acetate