反应详情

温度

0 °C

To a solution of 0.50 g of (RS)-1-(2,2-diethoxyethyl)-3-(hydroxycarbonylmethyl)-3-(N'-(3-methoxyphenyl)ureido)indolin-2-one in 50 ml of dichloromethane were added successively 0.140 g of 4-dimethylaminopyridine and 0.090 ml of thionyl chloride at 0° C., followed by stirring at 0° C. for 30 minutes. To the mixture were further added 0.140 g of 4-dimethylaminopyridine and 0.190 g of 4-methoxyaniline at 0° C. The resulting mixture was stirred at room temperature for 1 hour, and then washed with an aqueous solution of sodium chloride. The organic layer was dried over anhydrous sodium sulfate and concentrated. The crude product was purified by silica gel column chromatography (hexane/ethyl acetate=2/1) to give 0.54 g (88%) of the title compound.

1. customat 0° C
2. stirringThe resulting mixture was stirred at room temperature for 1 hour
3. washwashed with an aqueous solution of sodium chloride
4. dry with materialThe organic layer was dried over anhydrous sodium sulfate
5. concentrationconcentrated
6. customThe crude product was purified by silica gel column chromatography (hexane/ethyl acetate=2/1)