Benzoyl chloride → HCID 23320196、化合物

反応式

[NH2:1][CH2:2][CH2:3][CH2:4][N:5]1[CH2:10][CH2:9][N:8]([CH:11]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[C:12]2[CH:17]=[CH:16][C:15]([Cl:18])=[CH:14][CH:13]=2)[CH2:7][CH2:6]1.C(N(CC)CC)C.[C:32](Cl)(=[O:39])[C:33]1[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=1.[C:41]([OH:48])(=[O:47])/[CH:42]=[CH:43]/[C:44]([OH:46])=[O:45]>C(Cl)(Cl)Cl>[C:41]([OH:48])(=[O:47])/[CH:42]=[CH:43]/[C:44]([OH:46])=[O:45].[C:32]([NH:1][CH2:2][CH2:3][CH2:4][N:5]1[CH2:10][CH2:9][N:8]([CH:11]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[C:12]2[CH:17]=[CH:16][C:15]([Cl:18])=[CH:14][CH:13]=2)[CH2:7][CH2:6]1)(=[O:39])[C:33]1[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=1

参加物

実験手順

To a solution of 1-(3-aminopropyl)-4-(4-chlorobenzhydryl)piperazine (1.7 g) and triethylamine (0.7 g) in chloroform (20 ml) was dropwise added benzoyl chloride (0.7 ml) at ambient temperature and the mixture was stirred at the same temperature for 1.5 hours. The reaction mixture was washed successively with aqueous sodium bicarbonate and water, and then extracted with 10% hydrochloric acid. After neutralizing the aqueous extract with aqueous sodium carbonate, the desired product was extracted with ethyl acetate. The organic extract was washed with water, dried and evaporated in vacuo to give an oil. According to a conventional manner, the oily product was converted to fumaric acid salt, which was recrystallized from a mixture of ethanol and diethyl ether to afford 1-(3-benzoylaminopropyl)-4-(4-chlorobenzhydryl)piperazine fumarate (0.82 g) as white crystals. mp: 173°-175° C. (dec.).