反应详情

70 ml of ethanol and 15 ml of carbon disulfide were added to 2.6 g of 3,4-diaminoanisole and then a solution of 1.5 g of sodium hydroxide in 5 ml of water was added thereto. After heating with a water bath for 3.5 hours, the mixture was cooled with ice, filtered and then the solvent in the filtrate was distilled off under reduced pressure. The residue was dissolved in ethanol. The solution was filtrated to remove the insoluble matter and then the solvent in the filtrate was distilled off under reduced pressure. The residue was recrystallized from water-containing methanol to obtain 2.0 g of the titled compound (13).

1. temperatureAfter heating with a water bath for 3.5 hours
2. temperaturethe mixture was cooled with ice
3. filtrationfiltered
4. distillationthe solvent in the filtrate was distilled off under reduced pressure
5. dissolutionThe residue was dissolved in ethanol
6. filtrationThe solution was filtrated
7. customto remove the insoluble matter
8. distillationthe solvent in the filtrate was distilled off under reduced pressure
9. customThe residue was recrystallized from water-
10. additioncontaining methanol