反应详情

To a stirring suspension of ethyl-2-cyano-2-phenylacetate (10.34 g) and benzylhydrazine dihydrochloride (14.87 g) in ethanol (200 ml) at room temperature was added triethylamine (21.27 ml). The reaction mixture was heated to reflux for 24 hours. The solvent was removed under reduced pressure to yield the crude material as a brown oil. This was re-dissolved in ethyl acetate (100 ml) and washed with water (2×75 ml), then dried (MgSO4) and the solvent removed in vacuo to yield a pale brown oil. This was recrystallised from methanol to yield the title product as pale yellow crystals (2.5 g, ca. 20%)

1. temperatureThe reaction mixture was heated
2. temperatureto reflux for 24 hours
3. customThe solvent was removed under reduced pressure
4. customto yield the crude material as a brown oil
5. washwashed with water (2×75 ml)
6. dry with materialdried (MgSO4)
7. customthe solvent removed in vacuo
8. customto yield a pale brown oil
9. customThis was recrystallised from methanol