반응 #2331992

ord-f30ae14c4f7a4a518bae9a85934bd6c1

용매

반응 조건

온도
20°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타17 h, the solvent was evaporated under reduced pressure and water
  2. 2
    workup.ADDITIONwas added to the residue
  3. 3
    여과The resulting precipitate was filtered
  4. 4
    세척washed with water
  5. 5
    기타to give

실험 절차

A solution of 4-chloro-1-methyl-3-nitro-1H-[1,8]naphthyridin-2-one (1.54 g, 6.43 mmol) (J. Med. Chem. 1992, 35, 2863-2870) in 40 mL of THF was treated with 7.2 mL of 28% aqueous ammonia (6.4 g, 51 mmol). After stirring at 20° C. 17 h, the solvent was evaporated under reduced pressure and water was added to the residue. The resulting precipitate was filtered and washed with water to give to give 4-amino-1-methyl-3-nitro-1H-[1,8]naphthyridin-2-one (1.35 g, 96% yield). 1H-NMR (DMSO): δ 8.74 (m, 2H), 8.35 (s, 2H), 7.38 (dd, 1H, J=8.0, 4.8 Hz), 3.58 (s, 3H).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07678909B1uspto-grants-2010_03