Hydrogen chloride-ethyl acetate → HCID 22013762, compound
Reaction equation
[ClH:1].C(OCC)(=O)C.[CH3:8][N:9]([CH3:47])[CH2:10][CH2:11][CH2:12][N:13]1[C:17]2[CH:18]=[CH:19][C:20]([C:22]([NH:24][CH3:25])=[O:23])=[CH:21][C:16]=2[N:15]=[C:14]1[CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][CH2:43][CH2:44][CH2:45][CH3:46]>C(OCC)(=O)C.C(O)C>[ClH:1].[CH3:47][N:9]([CH3:8])[CH2:10][CH2:11][CH2:12][N:13]1[C:17]2[CH:18]=[CH:19][C:20]([C:22]([NH:24][CH3:25])=[O:23])=[CH:21][C:16]=2[N:15]=[C:14]1[CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][CH2:43][CH2:44][CH2:45][CH3:46]Participants
5
Reactant 2
Product 1
Reagents, catalysts & solvents 2
Procedure
4N Hydrochloric acid/ethyl acetate solution (0.89 ml) was added to a solution containing 1-[3-(dimethylamino)propyl]-2-henicosyl-N-methyl-1H-benzimidazole-5-carboxamide (1.818 g) in a mixture of ethyl acetate (18 ml) and ethanol (1.8 ml). After being stirred for 30 minutes at room temperature, the reaction mixture was concentrated. The residue was recrystallized with the mixed solution of ethyl acetate-ethanol, thereby yielding the entitled compound (1.611 g) as white crystals.
Workup
- concentrationthe reaction mixture was concentrated
- customThe residue was recrystallized with the mixed solution of ethyl acetate-ethanol
Sources & evidence
- ORD record
- ord-7c4bd62862fc49ad97d6b1d408b68261
- Source dataset
- uspto-grants-2001_03
- Patent number
- US06204264B1
Reaction notes
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