反应详情

To a solution of EXAMPLE 5B (1.25 g) in toluene (12 mL) was added Lawesson's reagent (1.212 g) and the mixture heated at reflux for 5 hours. After cooling, the solid was filtered and the filtrate concentrated. The residue was dissolved in ethyl acetate and the solution washed with 5% aqueous citric acid and brine. The organic layer was dried over magnesium sulfate, filtered, and concentrated, and the residue purified by flash chromatography on silica gel using 4:6 to 6:4 dichloromethane/hexane to afford the title compound.

1. temperaturethe mixture heated
2. temperatureat reflux for 5 hours
3. temperatureAfter cooling
4. filtrationthe solid was filtered
5. concentrationthe filtrate concentrated
6. dissolutionThe residue was dissolved in ethyl acetate
7. washthe solution washed with 5% aqueous citric acid and brine
8. dry with materialThe organic layer was dried over magnesium sulfate
9. filtrationfiltered
10. concentrationconcentrated
11. customthe residue purified by flash chromatography on silica gel using 4:6 to 6:4 dichloromethane/hexane