反应详情

A mixture of 4-bromophenylhydrazine hydrochloride (2.23 g, 10 mmol) and ethyl levulinate (1.58 g, 11 mmol) in 10 mL HOAc was heated to reflux for 20 h. The HOAc was removed under vaccum. The residue was dissolved in 10 mL EtOH. A solution of HCl in dioxane (12 mmol, 4M solution) was added. The mixture was heated to reflux for 4 h. The mixture was concentrated under vacuum and the residue was purified by flash chromatography on silica gel, eluting with 20% EtOAc in hexane to afford 2.1 g (78%) of the title compound.

1. temperaturewas heated
2. temperatureto reflux for 20 h
3. customThe HOAc was removed under vaccum
4. dissolutionThe residue was dissolved in 10 mL EtOH
5. temperatureThe mixture was heated
6. temperatureto reflux for 4 h
7. concentrationThe mixture was concentrated under vacuum
8. customthe residue was purified by flash chromatography on silica gel
9. washeluting with 20% EtOAc in hexane