反应详情

A cooled solution of 4′-aminoacetophenon (10 mmol) in pyridine (10 mL) at 0° C. was treated with methanesulfonyl chloride (15 mmol) and stirred at room temperature for 2 h. The reaction mixture was diluted with H2O and extracted with EtOAc several times. The combined organic layers were washed with H2O and brine, dried over MgSO4, filtered, and the filtrate was concentrated in vacuo. The residue was purified by flash column chromatography on silica gel using EtOAc:hexanes to afford 4′-(Methylsulfonylamino)acetophenone (13-5, LJO-298).

1. extractionextracted with EtOAc several times
2. washThe combined organic layers were washed with H2O and brine
3. dry with materialdried over MgSO4
4. filtrationfiltered
5. concentrationthe filtrate was concentrated in vacuo
6. customThe residue was purified by flash column chromatography on silica gel