Hydrochloric Acid → Dibenzo[b,f][1,4]thiazepin-11-ylamine hydrochloride
Reaction equation
[ClH:1].[CH:2]1[C:7]2[C:8]([NH2:17])=[N:9][C:10]3[CH:16]=[CH:15][CH:14]=[CH:13][C:11]=3[S:12][C:6]=2[CH:5]=[CH:4][CH:3]=1>CC(O)C.C(O)(C)C.COC(C)(C)C>[ClH:1].[CH:2]1[C:7]2[C:8]([NH2:17])=[N:9][C:10]3[CH:16]=[CH:15][CH:14]=[CH:13][C:11]=3[S:12][C:6]=2[CH:5]=[CH:4][CH:3]=1Participants
5
Procedure
A solution of gaseous HCl in i-PrOH (5.7 g, 31 wt-%) was added dropwise under stirring to a solution of dibenzo[b,f][1,4]thiazepin-11-ylamine (10.6 g) dissolved in a isopropanol/tert-butyl methyl ether (TBME) mixture (150 ml/120 ml). Stirring was continued for 1 h and the formed precipitate was filtered off, washed with tert-butyl methyl ether (TBME) and dried on air to obtain the desired compound as a colorless solid (11.2 g, 91%).
Workup
- filtrationthe formed precipitate was filtered off
- washwashed with tert-butyl methyl ether (TBME)
- customdried on air
Sources & evidence
- ORD record
- ord-79876ac24f6346eb98e31d846d8fd968
- Source dataset
- uspto-grants-2013_04
- Patent number
- US08420807B2
Reaction notes
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