反应详情

温度

90 °C

Into the same reactor as in Example 1 were charged 1.5 mg of palladium acetate, 0.83 g of 1,3-diiodo-5,5-dimethylhydantoin, 1.0 g of methyl 2-(1,1-dimethyl-2-methylsulfinylethylaminocarbonyl)benzoate and 5 ml of N-methylpyrrolidone. The mixture thus obtained was heated with stirring at 90° C. for 2 hours. After completion of the reaction, the reaction mixture was cooled to room temperature and poured into water, and the objective product was extracted with ethyl acetate. The organic layer was washed successively with aqueous solution of sodium thiosulfate and saturated aqueous solution of sodium chloride and dried over anhydrous magnesium sulfate. By distilling off the solvent under reduced pressure, a crude product was obtained. Purification of the crude product by silica gel column chromatography (ethyl acetate/n-hexane=1/3) gave 1.27 g of methyl 3-iodo-2-(1,1-dimethyl-2-methylsulfinylethylaminocarbonyl)-benzoate (yield 89.1%, melting point 150.7–151.8° C.).

1. customThe mixture thus obtained
2. temperaturewas heated
3. customAfter completion of the reaction
4. temperaturethe reaction mixture was cooled to room temperature
5. extractionthe objective product was extracted with ethyl acetate
6. washThe organic layer was washed successively with aqueous solution of sodium thiosulfate and saturated aqueous solution of sodium chloride
7. dry with materialdried over anhydrous magnesium sulfate
8. distillationBy distilling off the solvent under reduced pressure
9. customa crude product was obtained
10. customPurification of the crude product by silica gel column chromatography (ethyl acetate/n-hexane=1/3)