Hydrochloric Acid → HCID 18770445, compound
Reaction equation
[ClH:1].[Cl:2][C:3]1[CH:8]=[CH:7][C:6](/[CH:9]=[CH:10]/[CH:11]=[CH:12]/[C:13]([N:15]2[CH2:20][CH2:19][N:18]([CH2:21][CH:22]3[CH2:27][CH2:26][CH:25]([CH2:28][N:29]4[CH2:34][CH2:33][N:32]([C:35](=[O:47])/[CH:36]=[CH:37]/[CH:38]=[CH:39]/[C:40]5[CH:45]=[CH:44][C:43]([Cl:46])=[CH:42][CH:41]=5)[CH2:31][CH2:30]4)[CH2:24][CH2:23]3)[CH2:17][CH2:16]2)=[O:14])=[CH:5][CH:4]=1>C(O)C>[ClH:2].[ClH:1].[Cl:46][C:43]1[CH:42]=[CH:41][C:40](/[CH:39]=[CH:38]/[CH:37]=[CH:36]/[C:35]([N:32]2[CH2:33][CH2:34][N:29]([CH2:28][CH:25]3[CH2:26][CH2:27][CH:22]([CH2:21][N:18]4[CH2:19][CH2:20][N:15]([C:13](=[O:14])/[CH:12]=[CH:11]/[CH:10]=[CH:9]/[C:6]5[CH:5]=[CH:4][C:3]([Cl:2])=[CH:8][CH:7]=5)[CH2:16][CH2:17]4)[CH2:23][CH2:24]3)[CH2:30][CH2:31]2)=[O:47])=[CH:45][CH:44]=1Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
Concentrated hydrochloric acid (0.030 ml; 0.36 mmol) was added to a solution in ethanol (5 ml) of the crude crystals (72 mg; 0.090 mmol) of 1,4-bis[[4-[(E,E)-5-(4-chlorophenyl)-2,4-pentadienoyl]-1-piperazinyl]methyl]-cyclohexane 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 66 mg (yield: 50%) of 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-2b01e09d35af4bacaffe423632e1faa6
- Source dataset
- uspto-grants-2002_09
- Patent number
- US06448242B1
Reaction notes
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