反应详情

To a stirred soluition of 4,4,4-trifluoro-1-[4-(2-furyl)-3-methylphenyl]butane-1,3-dione (0.53 g, 1.80 mmol) in ethanol (22.5 ml) was added (4-sulfamoylphenyl)hydrazine hydrochloride (0.44 ml, 1.98 mmol), and the mixture was heated at reflux temperature for 16 hours. The mixture was cooled down to room temperature, and concentrated in vacuo. The residue was dissolved in ethyl acetate. washed with brine, dried over MgSO4, and concentrated in vacuo. The residue was purified by flash chromatography eluting with ethyl acetate/hexane (1/3). The resulting solid was recrystallized with dichloromethane-hexane to give the title compound (0.16 g, 20% yield).

1. temperaturethe mixture was heated
2. temperatureat reflux temperature for 16 hours
3. concentrationconcentrated in vacuo
4. dissolutionThe residue was dissolved in ethyl acetate
5. washwashed with brine
6. dry with materialdried over MgSO4
7. concentrationconcentrated in vacuo
8. customThe residue was purified by flash chromatography
9. washeluting with ethyl acetate/hexane (1/3)
10. customThe resulting solid was recrystallized with dichloromethane-hexane