反应详情

Heat a solution of 2,5-dibromo-3-methyl-pyridine (Chontech Inc.) (12.6 g, 50.3 mmol), piperazine-1-carboxylic acid tert-butyl ester (11.7 g, 62.9 mmol) and DIEA (13.3 g, 102.0 mmol) in DMA at 130° C. for 36 h. Partition the dark brown reaction mixture between water and EtOAc. Wash the EtOAc layer with water (1×) and brine (1×), dry (Na2SO4) and concentrate under reduced pressure to give the crude product. Purify by flash chromatography, eluting with 9:1 hexanes:EtOAc, increasing to 3:1 hexanes:EtOAc to provide the title compound as a solid.

1. customPartition the dark brown reaction mixture between water and EtOAc
2. washWash the EtOAc layer with water (1×) and brine (1×)
3. dry with materialdry (Na2SO4)
4. concentrationconcentrate under reduced pressure
5. customto give the crude product
6. customPurify by flash chromatography
7. washeluting with 9:1 hexanes
8. temperatureEtOAc, increasing to 3:1 hexanes