HCID 12268147, compound → HCID 21525725, compound
Reaction equation
[ClH:1].N[N:3]1[C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][C:8]=2[CH2:7][CH2:6][C:5]2[CH:14]=[CH:15][CH:16]=[CH:17][C:4]1=2.Cl.O.[C:20]1([N:26]2[CH2:31][CH2:30][N:29]([CH2:32][CH2:33][CH2:34][C:35](=O)[CH3:36])[CH2:28][CH2:27]2)[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1>>[ClH:1].[C:20]1([N:26]2[CH2:27][CH2:28][N:29]([CH2:32][CH2:33][C:34]3[C:17]4[C:4]5=[C:5]([CH:14]=[CH:15][CH:16]=4)[CH2:6][CH2:7][C:8]4[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=4[N:3]5[C:35]=3[CH3:36])[CH2:30][CH2:31]2)[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1Participants
Procedure
A suspension of 5-amino-10,11-dihydro-5H-dibenz[b,f]azepine hydrochloride (5.0g.) and 5-(4-phenyl-1-piperazinyl)-2-pentanone monohydrate monohydrochloride (6.2g.) in absolute alcohol (100 ml.) was heated on a water bath at 50° to 60°C. in a nitrogen atmosphere for one hour. The mixture was cooled and the solids were collected by filtration, washed with ethyl alcohol, suspended in aqueous methyl alcohol, collected by filtration, washed with water, ethyl alcohol and ether to give 2-[(4-phenyl-1-piperazinyl)-ethyl]-1-methyl-6,7-dihydroindolo-[1,7-ab][1]benzazepine hydrochloride (4.4g.), m.p. 280°-288°C.(dec.). By treatment of this hydrochloride salt in water with an equivalent of ammonium hydroxide and isolation using standard procedures there is obtained the free base 2-[(4-phenyl-1-piperazinyl)-ethyl]-1-methyl-6,7-dihydroindolo[1,7-ab][1]benzazepine.
Workup
- temperaturewas heated on a water bath at 50° to 60°C. in a nitrogen atmosphere for one hour
- temperatureThe mixture was cooled
- filtrationthe solids were collected by filtration
- washwashed with ethyl alcohol
- filtrationcollected by filtration
- washwashed with water, ethyl alcohol and ether
Sources & evidence
- ORD record
- ord-6d05e6a5b9bf4cd3b2e012aa35b89522
- Source dataset
- uspto-grants-1976_06
- Patent number
- US03966762
Reaction notes
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