反应详情

温度

0 °C

To a 100-mL round-bottomed flask was added 2-((2-methoxy-4-pyridinyl)methyl)piperazine (350 mg, 1.69 mmol), triethylamine (0.353 mL, 2.54 mmol), and 2-thiophenesulfonyl chloride (0.34 mL, 1.86 mmol, Aldrich, St. Louis, Mo.) in DCM (5 mL). The reaction mixture was stirred at 0° C. for 30 min. The reaction mixture was diluted with saturated NaHCO3 (10 mL) and extracted with EtOAc (2×40 mL). The organic extract was washed with saturated NaCl (5 mL) and dried over Na2SO4. The solution was filtered and concentrated in vacuo to give the crude material as light-yellow oil. The crude product was purified by silica gel chromatography, eluting with 10% MeOH/EtOAc to give 3-((2-methoxy-4-pyridinyl)methyl)-1-(2-thiophenylsulfonyl)piperazine (198 mg) as colorless glass.

1. extractionextracted with EtOAc (2×40 mL)
2. extractionThe organic extract
3. washwas washed with saturated NaCl (5 mL)
4. dry with materialdried over Na2SO4
5. filtrationThe solution was filtered
6. concentrationconcentrated in vacuo
7. customto give the crude material as light-yellow oil
8. customThe crude product was purified by silica gel chromatography
9. washeluting with 10% MeOH/EtOAc