Hydrochloric Acid → n-[1-(4-Phenylbutan-1-yl)piperidin-4-yl]-5-thia-1,8b-diazaacenaphthylene-4-carboxamide dihydrochloride
Reaction equation
[C:1]1([CH2:7][CH2:8][CH2:9][CH2:10][N:11]2[CH2:16][CH2:15][CH:14]([NH:17][C:18]([C:20]3[S:30][C:29]4[N:31]5[C:22](=[CH:23][N:24]=[C:25]5[CH:26]=[CH:27][CH:28]=4)[CH:21]=3)=[O:19])[CH2:13][CH2:12]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[ClH:32]>C(O)C>[ClH:32].[ClH:32].[C:1]1([CH2:7][CH2:8][CH2:9][CH2:10][N:11]2[CH2:12][CH2:13][CH:14]([NH:17][C:18]([C:20]3[S:30][C:29]4[N:31]5[C:22](=[CH:23][N:24]=[C:25]5[CH:26]=[CH:27][CH:28]=4)[CH:21]=3)=[O:19])[CH2:15][CH2:16]2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
To a solution of 437.4 mg (1.01 mM) of N-[1-(4-phenylbutan-1-yl)piperidin-4-yl]-5-thia-1,8b-diazaacenaphthylene-4-carboxamide in ethanol (10 ml) was added 0.5 ml (6 mM) of 12N-hydrochloric acid and the mixture was stirred at room temperature for 16 hours. After this reaction mixture was concentrated, a small amount of ethanol was added to the residue and the crystals were collected by filtration and rinsed with ethanol and diethyl ether to provide the title compound as orange-colored crystals.
Workup
- concentrationAfter this reaction mixture was concentrated
- additiona small amount of ethanol was added to the residue
- filtrationthe crystals were collected by filtration
- washrinsed with ethanol and diethyl ether
Sources & evidence
- ORD record
- ord-9d39209ff08e4d5e9c725ff1e862dc45
- Source dataset
- uspto-grants-2001_05
- Patent number
- US06235731B1
Reaction notes
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