Hydrochloric Acid → HCID 67711955, compound
Reaction equation
Br.[NH2:2][C:3]1[N:4]([CH2:20][C:21](=O)[C:22]([CH3:25])([CH3:24])[CH3:23])[C:5]2[CH:19]=[CH:18][CH:17]=[CH:16][C:6]=2[N+:7]=1[CH2:8][CH2:9][N:10]1[CH2:15][CH2:14][O:13][CH2:12][CH2:11]1.[OH-].[NH4+].[ClH:29]>>[ClH:29].[C:22]([C:21]1[N:2]=[C:3]2[N:4]([CH:20]=1)[C:5]1[CH:19]=[CH:18][CH:17]=[CH:16][C:6]=1[N:7]2[CH2:8][CH2:9][N:10]1[CH2:15][CH2:14][O:13][CH2:12][CH2:11]1)([CH3:25])([CH3:24])[CH3:23]Participants
4
Procedure
The hydrobromide obtained in Step A is heated at reflux in concentrated hydrochloric acid for 30 minutes. The solution is cooled and neutralised with an aqueous ammonium hydroxide solution. The reaction mixture is extracted with benzene and the extract is dried over sodium sulfate. Subsequently, pass through a stream of gaseous hydrochloric acid until acidity. The resulting precipitate is filtered and recrystallised from ethanol.
Workup
- temperatureThe solution is cooled
- extractionThe reaction mixture is extracted with benzene
- dry with materialthe extract is dried over sodium sulfate
- filtrationThe resulting precipitate is filtered
- customrecrystallised from ethanol
Sources & evidence
- ORD record
- ord-85242c788d704bda9f32d11196169e8c
- Source dataset
- uspto-grants-1997_04
- Patent number
- US05623073
Reaction notes
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