반응 #50137
ord-add641abc96540deb9dda91baff95149
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상세 조건
See reaction.notes.procedure_details.
후처리
- 1workup.DISTILLATIONThe solvent is distilled off
- 2workup.ADDITIONto the resulting residue is added chloroform
- 3세척the mixture is washed
- 4기타dried
- 5기타evaporated
- 6기타to remove the solvent
- 7기타The residue is purified by silica gel column chromatography (solvent; chloroform/ethanol=10:1)
실험 절차
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)