反应详情

After 1.09 g of Compound 4 obtained in Example 4 was dissolved in 10 ml of toluene, 1.07 g of Lawesson's reagent was added to the solution. The mixture was heated under reflux for an hour. The reaction mixture was allowed to stand at room temperature, and concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography [eluent: hexane-ethyl acetate (2:1 )]to obtain 1.46 g of a crude product. The crude product was recrystallized from ethyl acetate-hexane to obtain 1.09 g of Compound 36.

1. temperatureThe mixture was heated
2. temperatureunder reflux for an hour
3. customto stand at room temperature
4. concentrationconcentrated under reduced pressure
5. customThe resulting residue was purified by silica gel column chromatography [eluent
6. customhexane-ethyl acetate (2:1 )]to obtain 1.46 g of a crude product
7. customThe crude product was recrystallized from ethyl acetate-hexane