Hydrochloric Acid → HCID 67314829、化合物
反応式
Cl.[C:2]([O:5][CH2:6][CH2:7][N:8]([CH2:20][C:21]1[CH:26]=[CH:25][C:24]([CH2:27][N:28]=CC2C=CC=CC=2)=[CH:23][CH:22]=1)[CH2:9][CH2:10][CH2:11][CH2:12][N:13]([CH2:17][CH2:18][CH3:19])[CH2:14][CH2:15][CH3:16])(=[O:4])[CH3:3]>C(O)C>[C:2]([O:5][CH2:6][CH2:7][N:8]([CH2:20][C:21]1[CH:26]=[CH:25][C:24]([CH2:27][NH2:28])=[CH:23][CH:22]=1)[CH2:9][CH2:10][CH2:11][CH2:12][N:13]([CH2:14][CH2:15][CH3:16])[CH2:17][CH2:18][CH3:19])(=[O:4])[CH3:3]参加物
4
反応条件
- 温度
- 0 °C
実験手順
362 ml of 2N hydrochloric acid was charged in a 2-liter four-necked flask and cooled to 0° C. The solution prepared by dissolving 32.8 g of {[4-(benzylidene)aminomethylbenzyl]-(4-dipropylaminobutyl)amino}ethyl acetate (8a) in 120 ml of ethanol was added dropwise to the flask for about 20 minutes, the mixture was stirred at room temperature for three hours. The resultant was extracted five times with 100 ml of toluene. After the addition of 400 ml of chloroform to the aqueous layer, 60 g of sodium carbonate was slowly added to the mixture while stirring to adjust to pH 9. The solution was subjected to phase separation and extracted again with 400 ml of chloroform. The chloroform layer was washed twice with 200 ml of a saturated sodium bicarbonate aqueous solution, washed twice with 200 ml of water, dried over anhydrous sodium sulfate, and concentrated, thereby obtaining 26.3 g of [(4-aminomethylbenzyl)-(4-dipropylaminobutyl)amino]ethyl acetate (14) (yield: 99%, GC: 95%).