反应详情

10.0 g (53.6 mmol) of 2-chloro-3'4'-dihydroxyacetophenone was dissolved in 100 ml of methanol, and then 5.90 g (53.6 mmol) of ammonium dithiocarbamate was added thereto. The mixture was stirred at room temperature for 30 minutes. The solvent was distilled off under reduced pressure. To the residue, water was added to adjust the mixture to pH2.0, and then the mixture was extracted twice with ethyl acetate. The extract was dried over anhydrous sodium sulfate and-then concentrated. The crystal residue was washed with diethyl ether to obtain 8.80 g (yield: 72.9%) of the above-identified compound.

1. distillationThe solvent was distilled off under reduced pressure
2. additionTo the residue, water was added
3. extractionthe mixture was extracted twice with ethyl acetate
4. dry with materialThe extract was dried over anhydrous sodium sulfate
5. concentrationconcentrated
6. washThe crystal residue was washed with diethyl ether