反応 #73019

ord-b250780443984b3d86370bce76de5511

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他was hydrogenated at 50 psi (3.5×105 Pa) overnight on a Parr apparatus
  2. 2
    ろ過The reaction mixture was filtered through CELITE
  3. 3
    ろ過filter agent, which
  4. 4
    洗浄was rinsed with methanol afterwards
  5. 5
    濃縮The filtrate was concentrated

実験手順

A mixture of 1-{[(3-nitro[1,5]naphthyridin-4-yl)amino]methyl}cyclohexanol (4.55 g, 15.1 mmol) and 5% platinum on carbon (0.50 g) in acetonitrile (100 mL) was hydrogenated at 50 psi (3.5×105 Pa) overnight on a Parr apparatus. The reaction mixture was filtered through CELITE filter agent, which was rinsed with methanol afterwards. The filtrate was concentrated to give 1-{[(3-amino[1,5]naphthyridin-4-yl)amino]methyl}cyclohexanol. The 1-{[(3-amino[1,5]naphthyridin-4-yl)amino]methyl}cyclohexanol was concentrated from chloroform several times to remove residual methanol and was used directly onto the next step.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08541438B2uspto-grants-2013_09