Water → HCID 12899470、化合物

反応式

[CH3:1][N:2]1[C:12]2[C:7](=[C:8]([OH:13])[CH:9]=[CH:10][CH:11]=2)[CH2:6][CH2:5][C:3]1=[O:4].[H-].[Na+].CN(C)[CH:18]=[O:19].Cl[CH2:22][CH:23]([OH:37])[CH2:24][N:25]1[CH2:30][CH2:29][N:28]([C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)[CH2:27][CH2:26]1.[OH2:38]>>[C:18]([OH:19])(=[O:37])[C:3]([OH:4])=[O:38].[CH3:1][N:2]1[C:12]2[C:7](=[C:8]([O:13][CH2:22][CH:23]([OH:37])[CH2:24][N:25]3[CH2:30][CH2:29][N:28]([C:31]4[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=4)[CH2:27][CH2:26]3)[CH:9]=[CH:10][CH:11]=2)[CH2:6][CH2:5][C:3]1=[O:4]

参加物

反応物 5

HCID 962Water

HCID 6228Dimethylformamide

HCID 24758Sodium hydride

HCID 1822025-Hydroxy-1-methyl-3,4-dihydroquinolin-2-one

HCID 10037974HCID 10037974、化合物

生成物 1

HCID 12899470HCID 12899470、化合物

実験手順

1.8 Grams of 1-methyl-5-hydroxy-3,4-dihydrocarbostyril and 1 g of NaH (50% in oil) are mixed with 30 ml of dimethylformamide. Then 2.6 g of 1-chloro-2-hydroxy-3-(4-phenylpiperazinyl)propane are added thereto at a room temperature and stirred at 70° to 80° C. for 3 hours. The reaction mixture is poured into water and the organic layer is extracted with chloroform. After removing chloroform by distillation, the thus obtained residue is dissolved in acetone and the pH of the solution is adjusted by adding an acetone solution of oxalic acid. The crystals precipitated are collected by filtration and recrystallized from methanol-acetone to obtain 2.8 g of 1-methyl-5-[2-hydroxy-3-(4-phenylpiperazinyl)-propoxy]-3,4-dihydrocarbostyril oxalate in the form of colorless crystals with a melting point of 220°-221° C. (decomp.).