反应详情

温度

210 °C

A mixture of 2-(2-ethoxybenzamido)-3-methylbenzamide (1.6 g, 0.0053 mol) and anhydrous zinc chloride (2.29 g, 0.016 mol) was heated at 210° C. for 5 minutes, then allowed to cool. The residue was dissolved in dichloromethane-methanol (90:10, 200 ml) and this solution washed with an aqueous solution of ethylenediamine tetraacetic acid disodium salt (12 g in 400 ml of water). The aqueous phase was then extracted with a mixture of dichloromethane-methanol (90:10, 2×50 ml) and the organic solutions combined, dried (Na2SO4) and evaporated under vacuum. The residue crystallized from ethanol to give the title compound as colourless needles (0.6 g, 40%), m.p. 177-180° C.

1. temperatureto cool
2. washthis solution washed with an aqueous solution of ethylenediamine tetraacetic acid disodium salt (12 g in 400 ml of water)
3. extractionThe aqueous phase was then extracted with a mixture of dichloromethane-methanol (90:10, 2×50 ml)
4. dry with materialdried (Na2SO4)
5. customevaporated under vacuum
6. customThe residue crystallized from ethanol