反应详情

A mixture of 2-chloro-5-nitropyridine (1.0 g, 6.3 mmol), (2S,5R)-2,5-dimethyl-piperazine-1-carboxylic acid tert-butyl ester (1.4 g, 6.3 mmol), and potassium carbonate (1.7 g, 13 mmol) was stirred in DMSO (5.0 mL, 70 mmol) at 100° C. overnight. The reaction mixture was filtered thru a silica gel pad, which was washed with EtOAc (200 mL). The filtrate was washed with water (2×10 mL), concentrated, and purified by silica gel chromatography (eluted with ethyl acetate/hexane=0 to 80%) to give the title intermediate (1.724 g, 81% yield) as a yellow solid.

1. filtrationThe reaction mixture was filtered thru a silica gel pad, which
2. washwas washed with EtOAc (200 mL)
3. washThe filtrate was washed with water (2×10 mL)
4. concentrationconcentrated
5. custompurified by silica gel chromatography (eluted with ethyl acetate/hexane=0 to 80%)