反应详情

温度

0 °C

3-Chloropropanesulfonyl chloride (1.0 g, 5.6 mmol) dissolved in CH2Cl2 (20 mL) and cooled to ˜0° C. was treated dropwise with a solution of 1-methylpiperazine (566 mg, 5.6 mmol) and Et3N (572 mg, 5.6 mmol) in CH2Cl2 (10 mL). Following complete addition, the mixture was allowed to warm to rt and stir an additional 2 h. The solvent was evaporated under reduced pressure, the residue triturated with EtOAc (30 mL), vacuum filtered and the solid washed well with EtOAc. The filtrate was concentrated under reduced pressure and the oil residue dried under high vacuum to give the title compound (1.27 g, 93%): 1H NMR (CDCl3) δ: 2.17-2.26 (2H, m), 2.49 (3H, s), 2.75-2.77 (4H, m), 3.02-3.07 (2H, m), 3.46-3.49 (4H, m), 3.60 (2H, t).

1. additionaddition
2. temperatureto warm to rt
3. customThe solvent was evaporated under reduced pressure
4. customthe residue triturated with EtOAc (30 mL), vacuum
5. filtrationfiltered
6. washthe solid washed well with EtOAc
7. concentrationThe filtrate was concentrated under reduced pressure
8. customthe oil residue dried under high vacuum