反应详情

温度

120 °C

A mixture of (3-amino-4-chlorophenoxy)acetic acid methyl ester (0.70 g), 2-(4-methanesulfonylbenzyl)-4-methyl-3-oxopentanoic acid ethyl ester (1.4 g), polyphosphoric acid (3.5 g) and dioxane (50 mL) was heated at 120° C. for 2 days. The mixture was cooled to room temperature, diluted with water and extracted with ethyl acetate. The combined extracts were dried over magnesium sulfate and the solvent removed under reduced pressure. The residue was purified by column chromatography on silica gel, eluting with a mixture of ethyl acetate and cyclohexane (1:1 by volume) to afford title compound. 0.79 g.

1. temperatureThe mixture was cooled to room temperature
2. extractionextracted with ethyl acetate
3. dry with materialThe combined extracts were dried over magnesium sulfate
4. customthe solvent removed under reduced pressure
5. customThe residue was purified by column chromatography on silica gel
6. washeluting with a mixture of ethyl acetate and cyclohexane (1:1 by volume)