反应详情

To a solution of compound 9 (40 mg, 0.090 mmol) in anhydrous toluene (5 mL) was added Lawesson's reagent (40 mg, 0.099 mmol) under a nitrogen atmosphere, the mixture was heated at reflux for 12 h. After cooling down, the solvent was removed by evaporation in vacuo and the resulting residue was purified by column chromatography on silica gel (petroleum ether:EtOAc=3:1) to give compound 10 (30 mg, 73%) as a white solid. LC-MS tR=1.420 min in 2 min chromatography, MS (ESI) m/z 459.1 [M+H]+.

1. temperaturethe mixture was heated
2. temperatureat reflux for 12 h
3. temperatureAfter cooling down
4. customthe solvent was removed by evaporation in vacuo
5. customthe resulting residue was purified by column chromatography on silica gel (petroleum ether:EtOAc=3:1)