反应详情

A mixture of 2,4-dichloro-6-methyl-3-nitro-pyridine (Chorvat, Robert J. et al., J. Med. Chem., 1999, 42, 833., 7.5 g, 36.2 mmol), [2-(4-amino-phenyl)-ethyl]-carbamic acid tert-butyl ester (Stark, Peter A. et al., J. Med. Chem., 1992, 35, 4264., 1.14 g, 4.83 mmol) in N,N-diisopropylethylamine (50 ml) was heated at reflux temperature for 16 h. After cooling, the mixture was concentrated. The residue was diluted with dichloromethane (200 ml) and washed with saturated aqueous NaHCO3 solution (50 ml×2). The organic layer was dried (MgSO4), and concentrated. Purification by flash column chromatography eluting with hexane/ethyl acetate (1:1) to afford 310 mg (16%) of the title compound as orange solids.

1. temperaturewas heated
2. temperatureat reflux temperature for 16 h
3. temperatureAfter cooling
4. concentrationthe mixture was concentrated
5. additionThe residue was diluted with dichloromethane (200 ml)
6. washwashed with saturated aqueous NaHCO3 solution (50 ml×2)
7. dry with materialThe organic layer was dried (MgSO4)
8. concentrationconcentrated
9. customPurification by flash column chromatography
10. washeluting with hexane/ethyl acetate (1:1)