Acetic Anhydride → Methyl 3-(4-{5-[amino(imino)methyl]pyridin-2-yl}phenoxy)-2,2-dimethylpropanoate acetate
反応式
[NH2:1][C:2](=[N:24]O)[C:3]1[CH:4]=[CH:5][C:6]([C:9]2[CH:23]=[CH:22][C:12]([O:13][CH2:14][C:15]([CH3:21])([CH3:20])[C:16]([O:18][CH3:19])=[O:17])=[CH:11][CH:10]=2)=[N:7][CH:8]=1.C(OC(=O)C)(=O)C>C(O)(=O)C>[C:16]([OH:18])(=[O:17])[CH3:15].[NH2:24][C:2](=[NH:1])[C:3]1[CH:4]=[CH:5][C:6]([C:9]2[CH:10]=[CH:11][C:12]([O:13][CH2:14][C:15]([CH3:20])([CH3:21])[C:16]([O:18][CH3:19])=[O:17])=[CH:22][CH:23]=2)=[N:7][CH:8]=1参加物
4
実験手順
In acetic acid (60 mL) was dissolved methyl 3-(4-{5-[amino(hydroxyimino)methyl]-pyridin-2-yl}phenoxy)-2,2-dimethylpropanoate (5.8 g), acetic anhydride (4 mL) was added to the solution and the mixture was stirred at room temperature for 2 hours. To the residue obtained by concentrating the mixture under reduced pressure were added methanol (300 mL) and tetrahydrofuran (70 mL), and 10% palladium carbon (1.2 g) was added to the mixture under nitrogen atmosphere. The atmosphere of the reaction mixture was made hydrogen atmosphere, and the mixture was stirred at room temperature for 2 hours. After replacing the atmosphere with nitrogen, the mixture was filtered using Celite. The filtrate was concentrated under reduced pressure, ether was added to the obtained residue to pulverize the solid, and the solid was collected by filtration and dried to obtain methyl 3-(4-{5-[amino(imino)methyl]pyridin-2-yl}-phenoxy)-2,2-dimethylpropanoate acetate (6.11 g).