Hydrochloric Acid → HCID 67314829、化合物
反応式
[C:1]([O:4][CH2:5][CH2:6][N:7]([CH2:26][CH2:27][CH2:28][CH2:29][N:30]([CH2:34][CH2:35][CH3:36])[CH2:31][CH2:32][CH3:33])[CH2:8][C:9]1[CH:14]=[CH:13][C:12]([CH2:15][N:16]=CC2C=CC(OC)=CC=2)=[CH:11][CH:10]=1)(=[O:3])[CH3:2].Cl>C(O)C>[C:1]([O:4][CH2:5][CH2:6][N:7]([CH2:8][C:9]1[CH:14]=[CH:13][C:12]([CH2:15][NH2:16])=[CH:11][CH:10]=1)[CH2:26][CH2:27][CH2:28][CH2:29][N:30]([CH2:31][CH2:32][CH3:33])[CH2:34][CH2:35][CH3:36])(=[O:3])[CH3:2]参加物
4
反応条件
- 温度
- 0 °C
実験手順
In a 50 ml recovery flask, 430 mg (0.867 mmol, 1.0 equivalent) of {(4-dipropylaminobutyl)-[4-(4-methoxybenzylidene)aminomethylbenzyl]}amino}ethyl acetate (30) was dissolved in 4.3 ml of ethanol. The solution was cooled to 0° C. After the dropwise addition of 4.3 ml of 2N hydrochloric acid over about five minutes, the mixture was stirred at 5° C. or less for 22 hours. The mixture was added with 4.3 ml of 2N hydrochloric acid at 0° C., stirred for three hours, and extracted five times with 25 ml of chloroform. The aqueous layer was slowly added with 50 ml of chloroform and 40 ml of a 3N sodium hydroxide aqueous solution to make the mixture basic, and the mixture was subjected to phase separation. The mixture was then extracted three times with 25 ml of chloroform. The extract was dried over anhydrous sodium sulfate, filtered, and concentrated, thereby obtaining 319 mg of [(4-aminomethylbenzyl)-(4-dipropylaminobutyl)amino]ethyl acetate (14) as a slightly yellow oily substance (yield: 98%). [HPLC: 95.9% (HPLC measurement conditions A)]