反应详情

To a stirred solution of 1.07 g (5.24 mmol) of 2,6-dichlorobenzothiazole in dry DMF (25 mL) was added 2.4 g of potassium carbonate (15.7 mmol) and 0.5 g of piperazine (5.8 mmol). The mixture was stirred at room temperature for 4 h. When the reaction was complete it was partitioned between EtOAc (150 mL) and water (50 mL) and separated. The aqueous layer was extracted with EtOAC (2×100 mL). The combined organic layers were then washed with water (2×25 mL), brine, dried over Na2SO4, and the solvent was removed under reduced pressure to give 1.33 g (100%) of desired product as a white solid. MS (electrospray): exact mass calculated for C11H12ClN3S, 253.04; m/z found, 254.0 [M+H]+.

1. customwas partitioned between EtOAc (150 mL) and water (50 mL)
2. customseparated
3. extractionThe aqueous layer was extracted with EtOAC (2×100 mL)
4. washThe combined organic layers were then washed with water (2×25 mL), brine
5. dry with materialdried over Na2SO4
6. customthe solvent was removed under reduced pressure