Methanol → HCID 69155736、化合物
反応式
Cl.[C:2]([C:5]1[CH:10]=[C:9]([CH2:11][O:12][C:13]([C:15]2[N:16]([CH2:33][C:34]3[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=3)[C:17](=[O:32])[C:18]3[C:23]([C:24]=2[C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)=[CH:22][C:21]([Br:31])=[CH:20][CH:19]=3)=[O:14])[CH:8]=[CH:7][N:6]=1)([OH:4])=[O:3].S(=O)(=O)(O)O.[CH3:45]O>>[CH3:45][O:3][C:2]([C:5]1[CH:10]=[C:9]([CH2:11][O:12][C:13]([C:15]2[N:16]([CH2:33][C:34]3[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=3)[C:17](=[O:32])[C:18]3[C:23]([C:24]=2[C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)=[CH:22][C:21]([Br:31])=[CH:20][CH:19]=3)=[O:14])[CH:8]=[CH:7][N:6]=1)=[O:4]参加物
4
実験手順
To a solution (3.0 ml) of 2-benzyl-6-bromo-1-oxo-4-phenyl-1,2-dihydroisoquinoline-3-carboxylic acid 2-carboxypyridin-4-ylmethyl ester hydrochloride (120 mg) in methanol was added conc. sulfuric acid (0.3 ml) at 0° C. with stirring, and the mixture was stirred at 50° C. for 48 hrs. After cooling the mixture, the solvent was removed under reduced pressure. The residue was partitioned between ethyl acetate and saturated aqueous sodium hydrogen carbonate, and the organic layer was dried over magnesium sulfate and concentrated under reduced pressure. The residue was purified by medium pressure preparative LC (hexane/ethyl acetate=4/1-1/1) to give the title compound (73 mg) as colorless crystals.