反应详情

A mixture of 4-dimethylamino-3-phenyl-3-butene-2-one (14.1 grams) and cyanoacetamide (5.9 grams) in 100 ml methanol was added to sodium methoxide (7.9 grams) in 100 ml methanol. The mixture was refluxed for 18 hours and then the crude reaction was stripped and the residue dissolved in a small amount of hot water. Acidification to pH 6-7 gave a gum-like solid which was collected by filtration. Further acidification to a lower pH gave only an oil. Trituration of the gum with ethyl acetate and chilling resulted in an off-white solid which was identified by NMR as the desired product, yield 2.8 grams, m.p. 280°-290° C.

1. temperatureThe mixture was refluxed for 18 hours
2. customthe crude reaction
3. customAcidification to pH 6-7 gave a gum-like solid which
4. filtrationwas collected by filtration
5. customFurther acidification to a lower pH gave only an oil
6. customresulted in an off-white solid which