反应详情

To a solution of 1-(3,5-dichloropyridin-4-yl)piperidine-4-carboxamide 23 (40 mg, 0.15 mmol) in THF (2 mL) was added Lawesson's reagent (71 mg, 0.18 mmol) and the mixture was heated at reflux for 2.5 h. After cooling to r.t. the mixture was poured into a saturated solution of sodium hydrogen carbonate (20 mL) and extracted with EtOAc (2×20 mL). The combined organic extracts were washed with water (20 mL), brine (20 mL), dried (MgSO4) and concentrated under reduced pressure. The crude product was purified by flash column chromatography on silica gel (CH2Cl2, MeOH, 99:1) to furnish the title compound as a white solid (21 mg, 40%), m/z (ESI) C11H14Cl2N2S requires 290.0280 found [M+H]+ 290.0280.

1. temperaturethe mixture was heated
2. temperatureat reflux for 2.5 h
3. extractionextracted with EtOAc (2×20 mL)
4. washThe combined organic extracts were washed with water (20 mL), brine (20 mL)
5. dry with materialdried (MgSO4)
6. concentrationconcentrated under reduced pressure
7. customThe crude product was purified by flash column chromatography on silica gel (CH2Cl2, MeOH, 99:1)