反应详情

Methyl 3,5-bis(dimethylcarbamoylthio)benzoate (3.42 g, 10 mmol) was made to react with 5% aqueous sodium hydroxide solution (10 ml. 12.5 mmol) for 3 hours at 22-25° C. with stirring. After cooling by the addition of 50 ml of ice-water, the reaction mixture was extracted with ethyl acetate (300 ml×3) and the extract was dried over magnesium sulfate. The ethyl acetate was evaporated under reduced pressure and the colorless crystals thus obtained was recrystallized from ethanol to give 2.86 g (87.2%) of 3,5-bis(dimethylcarbamoylthio)benzoic acid as colorless needles. The melting point is 196-198° C. (with decomposition).

1. extractionthe reaction mixture was extracted with ethyl acetate (300 ml×3)
2. dry with materialthe extract was dried over magnesium sulfate
3. customThe ethyl acetate was evaporated under reduced pressure
4. customthe colorless crystals thus obtained
5. customwas recrystallized from ethanol