Hydrochloric Acid → N-(1-benzylpiperidin-4-ylmethyl)-5-thia-1,8b-diazaacenaphthylene-4-carboxamide Dihydrochloride
Reaction equation
[CH2:1]([N:8]1[CH2:13][CH2:12][CH:11]([CH2:14][NH:15][C:16]([C:18]2[S:28][C:27]3[N:29]4[C:20](=[CH:21][N:22]=[C:23]4[CH:24]=[CH:25][CH:26]=3)[CH:19]=2)=[O:17])[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[ClH:30]>C(O)C>[ClH:30].[ClH:30].[CH2:1]([N:8]1[CH2:13][CH2:12][CH:11]([CH2:14][NH:15][C:16]([C:18]2[S:28][C:27]3[N:29]4[C:20](=[CH:21][N:22]=[C:23]4[CH:24]=[CH:25][CH:26]=3)[CH:19]=2)=[O:17])[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1Participants
4
Procedure
In a solution of 479 mg (1.18 mmol) of N-(1-benzylpiperidin-4-ylmethyl)-5-thia-1,8b-diazaacenaphthylene-4-carboxamide in ethanol (4 ml) was added 1.0 ml (4 mM) of 4N-HCl/methnol and the mixture was stirred at room temperature for several minutes. The solvent was then distilled off under reduced pressure and the residue was diluted with ethanol and diethyl ether. The resulting crystals were collected by filtration and rinsed with ethanol and diethyl ether to provide the title compound.
Workup
- distillationThe solvent was then distilled off under reduced pressure
- additionthe residue was diluted with ethanol and diethyl ether
- filtrationThe resulting crystals were collected by filtration
- washrinsed with ethanol and diethyl ether
Sources & evidence
- ORD record
- ord-b19b43e1783142e29dc42b5848319df9
- Source dataset
- uspto-grants-2001_05
- Patent number
- US06235731B1
Reaction notes
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