反应详情

温度

0 °C

A 500 mL round-bottomed flask was charged with (S)-2-methylpiperazine (10.23 g, 102 mmol, Sigma-Aldrich, St. Louis, Mo.) and 100 mL of CH2Cl2. After cooling to 0° C., 2-thiophenesulfonyl chloride (18.65 g, 102 mmol, Sigma-Aldrich, St. Louis, Mo.) was added. This mixture was stirred at 0° C. for 15 min then diluted with water (100 mL). The layers were separated and the organics were dried (MgSO4) and concentrated to give an oil. To this oil was added 300 mL of EtOAc and 28 mL of 4 M HCl in dioxane. The resulting white precipitate was collected by filtration to give (S)-2-methyl-4-(2-thiophenylsulfonyl)piperazine hydrochloride (26 g).

1. customThe layers were separated
2. dry with materialthe organics were dried (MgSO4)
3. concentrationconcentrated
4. customto give an oil
5. filtrationThe resulting white precipitate was collected by filtration