Hydrochloric Acid → 1,3-Bis[4-[4-(3,4,5-trimethoxyphenyl)benzoyl]-1-piperazinyl]propane dihydrochloride
Reaction equation
[ClH:1].[CH3:2][O:3][C:4]1[CH:5]=[C:6]([C:14]2[CH:56]=[CH:55][C:17]([C:18]([N:20]3[CH2:25][CH2:24][N:23]([CH2:26][CH2:27][CH2:28][N:29]4[CH2:34][CH2:33][N:32]([C:35](=[O:54])[C:36]5[CH:41]=[CH:40][C:39]([C:42]6[CH:47]=[C:46]([O:48][CH3:49])[C:45]([O:50][CH3:51])=[C:44]([O:52][CH3:53])[CH:43]=6)=[CH:38][CH:37]=5)[CH2:31][CH2:30]4)[CH2:22][CH2:21]3)=[O:19])=[CH:16][CH:15]=2)[CH:7]=[C:8]([O:12][CH3:13])[C:9]=1[O:10][CH3:11]>C(O)C>[ClH:1].[ClH:1].[CH3:49][O:48][C:46]1[CH:47]=[C:42]([C:39]2[CH:38]=[CH:37][C:36]([C:35]([N:32]3[CH2:33][CH2:34][N:29]([CH2:28][CH2:27][CH2:26][N:23]4[CH2:24][CH2:25][N:20]([C:18](=[O:19])[C:17]5[CH:55]=[CH:56][C:14]([C:6]6[CH:5]=[C:4]([O:3][CH3:2])[C:9]([O:10][CH3:11])=[C:8]([O:12][CH3:13])[CH:7]=6)=[CH:15][CH:16]=5)[CH2:21][CH2:22]4)[CH2:30][CH2:31]3)=[O:54])=[CH:41][CH:40]=2)[CH:43]=[C:44]([O:52][CH3:53])[C:45]=1[O:50][CH3:51]Participants
4
Procedure
Concentrated hydrochloric acid (0.015 ml; 0.18 mmol) was added to a solution of 1,3-bis[4-[4-(3,4,5-trimethoxyphenyl)benzoyl]-1-piperazinyl]propane (43 mg; 0.050 mmol) in ethanol (5 ml) and the reaction mixture was concentrated under reduced pressure. After a process of adding ethanol (10 ml) to the residue and concentrating the mixture under reduced pressure was performed twice, the resultant concentrated residue was recrystallized from methanoldiethyl ether to obtain the title compound as a colorless crystalline powder.
Workup
- concentrationthe reaction mixture was concentrated under reduced pressure
- concentrationAfter a process of adding ethanol (10 ml) to the residue and concentrating the mixture under reduced pressure
- customthe resultant concentrated residue was recrystallized from methanoldiethyl ether
Sources & evidence
- ORD record
- ord-38a22350c46f423ab9c37bec6b8bc793
- Source dataset
- uspto-grants-2002_09
- Patent number
- US06448242B1
Reaction notes
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