反応 #50137

ord-add641abc96540deb9dda91baff95149

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.DISTILLATIONThe solvent is distilled off
  2. 2
    workup.ADDITIONto the resulting residue is added chloroform
  3. 3
    洗浄the mixture is washed
  4. 4
    その他dried
  5. 5
    その他evaporated
  6. 6
    その他to remove the solvent
  7. 7
    その他The residue is purified by silica gel column chromatography (solvent; chloroform/ethanol=10:1)

実験手順

To a mixture of the compound obtained in Example 12 (1.70 g) and pyridine (20 ml) is added acetic anhydride (5 ml), and the mixture is stirred overnight. The solvent is distilled off, and to the resulting residue is added chloroform, and the mixture is washed, dried, and evaporated to remove the solvent. The residue is purified by silica gel column chromatography (solvent; chloroform/ethanol=10:1) to give methyl 2-n-butyl-5-acetyl-3-(2'-methoxycarbonylbiphenyl-4-yl)methyl-4,5,6,7-tetrahydroimidazo[4,5-c] pyridine-4-carboxylate (0.47 g) as an oil. NMR (CDCl3) δ: 0.88 (3H, t), 2.21 (3H, s), 3.46 (3H, s), 3.64 (3H, s), 5.33 (2H, ABq)

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05424316uspto-grants-1995_06