反应详情

温度

100 °C

A mixture of (3-amino-4-chlorophenoxy)acetic acid methyl ester (0.35 g), 3-(2-chloro-4-methanesulfonylbenzyl)pentane-2,4-dione (0.5 g) and polyphosphoric acid (5.0 g) was heated at 100° C. for 3.5 hours. The mixture was cooled to room temperature, diluted with water and extracted with ethyl acetate. The combined extracts were washed with water and saturated aqueous sodium chloride solution and dried over magnesium sulfate. The solvent was removed under reduced pressure and the residue purified by column chromatography on silica gel, eluting with a mixture of ethyl acetate and cyclohexane (2:8 to 3:7 by volume) to afford title compound as a pale yellow waxy solid, 0.36 g.

1. temperatureThe mixture was cooled to room temperature
2. extractionextracted with ethyl acetate
3. washThe combined extracts were washed with water and saturated aqueous sodium chloride solution
4. dry with materialdried over magnesium sulfate
5. customThe solvent was removed under reduced pressure
6. customthe residue purified by column chromatography on silica gel
7. washeluting with a mixture of ethyl acetate and cyclohexane (2:8 to 3:7 by volume)