Ammonium Chloride → Hydrochloric Acid
Reaction equation
[CH3:1][C:2]1[C:18]2[C:5]3=[C:6]([CH:15]=[CH:16][CH:17]=2)[CH2:7][CH2:8][C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[N:4]3[C:3]=1[CH2:19][CH2:20][NH:21][CH3:22].[Na].[Cl-:24].[NH4+]>O1CCCC1>[CH3:1][C@@H:2]1[C:18]2[C:5]3=[C:6]([CH:15]=[CH:16][CH:17]=2)[CH2:7][CH2:8][C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[N:4]3[C@H:3]1[CH2:19][CH2:20][NH:21][CH3:22].[ClH:24]Participants
6
Procedure
7.4 g (0.0255 mol) of 6,7-dihydro-2-methyl-1-(2-methylaminoethyl)-indolo[1,7-ab][1]benzazepine were dissolved in 74 ml of tetrahydrofuran (freshly distilled from sodium) and 148 ml of liquid ammonia and reduced with 1.17 g (2 × 0.0255 mol) of sodium. Addition of a further 0.12 g (10% excess) of sodium caused formation of a permanent blue colour. After decomposition with 3 g of ammonium chloride, the mixture was worked up in the manner described in part B of Example 2. The basic product was distilled at ca 150° C (air-bath temperature)/10-5 mm Hg to give the trans-1,2,6,7-tetrahydro-2-methyl-1-(2-methylaminoethyl)-indolo[1,7-ab][1]benzazepine whose hydrochloride melted at 198°-200° C.
Workup
- distillationfreshly distilled from sodium) and 148 ml of liquid ammonia
- distillationThe basic product was distilled at ca 150° C (air-bath temperature)/10-5 mm Hg
Sources & evidence
- ORD record
- ord-be5f51eff5c34ad08fc4e84959c53b90
- Source dataset
- uspto-grants-1976_11
- Patent number
- US03989717
Reaction notes
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