反应详情

3,6-dichloropyridazine (14.90 g, 100 mmol), sodium carbonate (10.60 g, 100 mmol) and DMA (80 mL) were placed in a 250 mL three-necked bottle, and the solution of 1-(3-hydroxypropyl)piperazine (14.4 g, 100 mmol) in DMA (20 mL) was added slowly in dropwise within 30 min under an ice-bath condition. The mixture was stirred at room temperature overnight, distilled under a reduced pressure to remove the solvent to obtain a brown solid, which was subjected to a column chromatography (gradient elution: petroleum/acetone system, v/v 2: 1 to acetone) to obtain a white solid, 13 g, yield 50.8%.

1. distillationdistilled under a reduced pressure
2. customto remove the solvent
3. customto obtain a brown solid, which
4. washwas subjected to a column chromatography (gradient elution: petroleum/acetone system, v/v 2: 1 to acetone)
5. customto obtain a white solid, 13 g, yield 50.8%