反应详情

温度

100 °C

A mixture of 52.0 g (30.5 mmol) 6-chloro-N-methyl-nicotinamide and 176 ml (1.58 mol) 1-methylpiperazine was heated at 100° C. for 1.5 h in an autoclave. After cooling to room temperature excess 1-methylpiperazine was removed by distillation. The residue was partitioned in 1000 ml dichloromethane/1 N aqueous sodium hydroxide solution. The layers were separated and the aqueous layer was extracted with three 500 ml portions of dichloromethane. Concentration and short column chromatography yielded 72.3 g (97%) of the title compound as a light brown solid.

1. customwas removed by distillation
2. customThe residue was partitioned in 1000 ml dichloromethane/1 N aqueous sodium hydroxide solution
3. customThe layers were separated
4. extractionthe aqueous layer was extracted with three 500 ml portions of dichloromethane
5. concentrationConcentration and short column chromatography