反应详情

To a solution of compound 9 (90 mg, 0.19 mmol) in anhydrous toluene (10 mL) was added Lawesson's reagent (84 mg, 0.20 mmol) under a nitrogen atmosphere, the mixture was heated to 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 eluting with petroleum ether:EtOAc (3:1) to give compound 10 (65 mg, 70%) as a white solid. LC-MS tR=1.503 min in 2 min chromatography, MS (ESI) m/z 483.1 [M+H]+.

1. temperaturethe mixture was heated
2. temperatureto 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 eluting with petroleum ether:EtOAc (3:1)