3-(p-Chlorobenzylamino)propyl(n-butyl)phosphinic acid ethyl ester → 3-(p-Chlorobenzylamino)propyl(n-butyl)phosphinic acid hydrochloride
反応式
C([O:3][P:4]([CH2:10][CH2:11][CH2:12][NH:13][CH2:14][C:15]1[CH:20]=[CH:19][C:18]([Cl:21])=[CH:17][CH:16]=1)([CH2:6][CH2:7][CH2:8][CH3:9])=[O:5])C>Cl>[ClH:21].[Cl:21][C:18]1[CH:17]=[CH:16][C:15]([CH2:14][NH:13][CH2:12][CH2:11][CH2:10][P:4]([CH2:6][CH2:7][CH2:8][CH3:9])(=[O:3])[OH:5])=[CH:20][CH:19]=1参加物
3
実験手順
A solution of 1.86 g of 3-(p-chlorobenzylamino)propyl(n-butyl)phosphinic acid ethyl ester in 30 ml of semi-concentrated hydrochloric acid is heated under reflux overnight, a clear solution forming after only 10 minutes. The solution is then cooled to 0°, whereupon a white precipitate forms. The precipitate is filtered off, washed with water and dried under reduced pressure at 60°. Recrystallisation from water and drying yield 3-(p-chlorobenzylamino)propyl(n-butyl)phosphinic acid hydrochloride having a melting point of 212-214°.