反应详情

To a solution of 2-(4-cyclopropylpiperazin-1-yl)benzothiazol-6-ylamine (500 mg, 1.82 mmol) in DMF (10 mL) was added NaH (220 mg, 5.46 mmol) at 0° C. The mixture was allowed to warm to rt and then stirred for 30 min. A solution of 3-chloropropane-1-sulfonyl chloride (450 mg, 2.55 mmol) in DMF (2 mL) was added and the reaction mixture was stirred for 2 h. The resulting mixture was extracted with ethyl acetate (3×20 mL). The combined organic extracts were dried (Na2SO4) and concentrated under reduced pressure to give a residue which was purified by column chromatography on silica gel (elute: 2% dichloromethane in methanol). This afforded 217 mg (31%) of 2-(4-cyclopropylpiperazin-1-yl)-6-(1,1-dioxo-1λ6-isothiazolidin-2-yl)benzothiazole.

1. stirringthe reaction mixture was stirred for 2 h
2. extractionThe resulting mixture was extracted with ethyl acetate (3×20 mL)
3. dry with materialThe combined organic extracts were dried (Na2SO4)
4. concentrationconcentrated under reduced pressure
5. customto give a residue which
6. customwas purified by column chromatography on silica gel (elute: 2% dichloromethane in methanol)