反应详情

温度

0 °C

To a 100-mL round-bottomed flask was added 2-(3-methoxybenzyl)piperazine (128 mg, 0.62 mmol), 5 mL of CH2Cl2, triethylamine (0.129 mL, 0.93 mmol) and 2-thiophenesulfonyl chloride (0.113 mL, 0.62 mmol, Aldrich, St. Louis, Mo.). The reaction mixture was stirred at 0° C. for 1 h and then diluted with aqueous saturated NaHCO3 (5 mL) and extracted with EtOAc (2×30 mL). The organic extracts were washed with saturated NaCl (10 mL) and dried over Na2SO4. The solution was filtered and concentrated in vacuo to give the crude material as a light-yellow oil. The crude product was purified by silica gel chromatography, eluting with 5% MeOH in EtOAc to give 3-(3-methoxybenzyl)-1-(thiophen-2-ylsulfonyl)piperazine as a colorless oil (162 mg).

1. extractionextracted with EtOAc (2×30 mL)
2. washThe organic extracts were washed with saturated NaCl (10 mL)
3. dry with materialdried over Na2SO4
4. filtrationThe solution was filtered
5. concentrationconcentrated in vacuo
6. customto give the crude material as a light-yellow oil
7. customThe crude product was purified by silica gel chromatography
8. washeluting with 5% MeOH in EtOAc