反应详情

6-Bromo-1,1-dioxo-1-thiochroman-4-one thiosemicarbazone (23) Into a round bottom flask containing 0.198 g of the appropriate thiochroman-4-one (0.147 g, 0.534 mmol), 10 mL of anhydrous methanol were added and the solution was refluxed for about 15 minutes before adding thiosemicarbazide (0.0598 g, 0.657 mmol) and 1.4 mg of TsOH. After the reaction mixture was refluxed under nitrogen atmosphere for 10 h, a solid was formed which was filtered and, then purified by column chromatography (30% EtOAc/70% hex). 0.0618 g (0.178 mmol) of the product was obtained in a 33% yield.

1. additionwere added
2. temperaturethe solution was refluxed for about 15 minutes
3. temperatureAfter the reaction mixture was refluxed under nitrogen atmosphere for 10 h
4. customa solid was formed which
5. filtrationwas filtered
6. custompurified by column chromatography (30% EtOAc/70% hex)