反应详情

1-(3-Methyl-5-nitro-pyridin-2-yl)-piperazine is prepared by heating a solution of 1 g of 2-chloro-3-methyl-5-nitro-pyridine (Maybridge Chemical Company Ltd.) and piperazine (5 g) in DMA at 110° C. for 16 h. Partition between EtOAc and water and wash the organic layer with water (2×). Dry the organic layer with Na2SO4 and concentrate to give crude product. Purify via flash chromatography eluting with MeOH:DCM:NH4OH (9:90:1) to give the title compound.

1. custom1-(3-Methyl-5-nitro-pyridin-2-yl)-piperazine is prepared
2. customPartition between EtOAc and water
3. washwash the organic layer with water (2×)
4. dry with materialDry the organic layer with Na2SO4
5. concentrationconcentrate
6. customto give crude product
7. customPurify via flash chromatography
8. washeluting with MeOH:DCM:NH4OH (9:90:1)