反应详情

A mixture of o-anisidine (22.6 ml, 0.2 mol), triethyl orthoformate (33.3 ml, 0.2 mol) and ethyl butyrylacetate (31.6 ml. 0.2 mol) was heated such that ethanol distilled over slowly. After 2.5 hours the mixture was allowed to cool, diluted with methanol (100 ml) and allowed to crystallise. The N-(2-methoxyphenyl)-2-butyryl-3-(2-methoxyphenylamino)acrylamide by-product was filtered off. Evaporation of the mother liquors and recrystallisation from petroleum ether (40-60) gave ethyl 2-butyryl-3-(2-methoxyphenylamino)acrylate (15.82 g, 27.2%), m.p. 74°-76°.

1. distillationdistilled over slowly
2. temperatureto cool
3. additiondiluted with methanol (100 ml)
4. customto crystallise
5. filtrationThe N-(2-methoxyphenyl)-2-butyryl-3-(2-methoxyphenylamino)acrylamide by-product was filtered off
6. customEvaporation of the mother liquors and recrystallisation from petroleum ether (40-60)