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 methanol-diethyl 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 methanol-diethyl ether
Sources & evidence
- ORD record
- ord-9af23574a180465390d653afe981d2a0
- Source dataset
- uspto-grants-2003_11
- Patent number
- US06645957B2
Reaction notes
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