反应详情

温度

0 °C

A 250 mL round-bottomed flask was charged with 2-(benzyloxymethyl)piperazine (2.10 g, 10.1 mmol), triethylamine (1.42 mL, 10.2 mmol) and CH2Cl2 (50 mL). After cooling to 0° C., 2-thiophenesulfonyl chloride (1.84 g, 10.1 mmol, Sigma-Aldrich, St. Louis, Mo.) was added slowly via syringe. After 2 h, the mixture was concentrated and diluted with EtOAc (200 mL). The organic solution was washed with 1 N HCl (2×50 mL) and the combined acidic layers made basic with Na2CO3. The resulting basic solution was extracted with EtOAc (3×100 mL) and the combined organic layers were dried (MgSO4), filtered and concentrated to give 3-(benzyloxymethyl)-1-(thiophen-2-ylsulfonyl)piperazine (1.79 g) as a yellow tar.

1. concentrationthe mixture was concentrated
2. additiondiluted with EtOAc (200 mL)
3. washThe organic solution was washed with 1 N HCl (2×50 mL)
4. extractionThe resulting basic solution was extracted with EtOAc (3×100 mL)
5. dry with materialthe combined organic layers were dried (MgSO4)
6. filtrationfiltered
7. concentrationconcentrated