HCID 22990107、化合物 → HCID 17824062、化合物
反応式
C(CC1C=CC([NH:10][C:11]([C:13]2[CH2:14][CH2:15][O:16][C:17]3[CH:23]=[CH:22][C:21]([C:24]4[CH:29]=[CH:28][C:27]([CH3:30])=[CH:26][CH:25]=4)=[CH:20][C:18]=3[CH:19]=2)=[O:12])=CC=1)#N>Cl.C(O)C.O1CCOCC1>[CH3:30][C:27]1[CH:26]=[CH:25][C:24]([C:21]2[CH:22]=[CH:23][C:17]3[O:16][CH2:15][CH2:14][C:13]([C:11]([NH2:10])=[O:12])=[CH:19][C:18]=3[CH:20]=2)=[CH:29][CH:28]=1参加物
3
実験手順
To N-(4-cyanomethylphenyl)-7-(4-methylphenyl)-2,3-dihydro-1-benzooxepine-4-carboxamide (789 mg) was added under ice cooling a solution of 24% hydrogen chloride/ethanol/dioxane (10 ml). The resulting mixture was stirred at room temperature for one hour and was then concentrated. To the residue suspended in ethanol (20 ml) was added ethylenediamine (0.4 ml) under ice cooling. The resulting mixture was stirred at room temperature for 15 hours, was then concentrated and was mixed with an aqueous solution of sodium bicarbonate. The resulting mixture was extracted with ethyl acetate, and the extract was washed with an aqueous solution of sodium chloride. After drying (magnesium sulfate), the extract was concentrated, and the residue was recrystallized from ethyl acetate/methanol to obtain N-(4-imidazolin-2-yl)methyl]phenyl]-7-(4-methylphenyl)-2,3-dihydro-1-benzooxepine-4-carboxamide (compound 94) (580 mg) as colorless crystals.