Hydrochloric Acid → HCID 86643317, Verbindung

Reaktionsgleichung

[CH3:1][N:2]([CH3:34])[CH2:3][CH2:4][CH2:5][C:6]1[CH:7]=[C:8]([NH:13][C:14]2[N:15]=[CH:16][C:17]3[CH2:18][C:19](=[S:33])[NH:20][C:21]4[CH:28]=[C:27]([C:29]([F:32])([F:31])[F:30])[CH:26]=[CH:25][C:22]=4[C:23]=3[N:24]=2)[C:9]([CH3:12])=[N:10][CH:11]=1.C(O)C.[ClH:38]>>[ClH:38].[ClH:38].[CH3:34][N:2]([CH3:1])[CH2:3][CH2:4][CH2:5][C:6]1[CH:7]=[C:8]([NH:13][C:14]2[N:15]=[CH:16][C:17]3[CH2:18][C:19](=[S:33])[NH:20][C:21]4[CH:28]=[C:27]([C:29]([F:32])([F:31])[F:30])[CH:26]=[CH:25][C:22]=4[C:23]=3[N:24]=2)[C:9]([CH3:12])=[N:10][CH:11]=1

Komponenten

Edukt 3

HCID 313Hydrochloric Acid

HCID 702Ethanol2×

HCID 46235922Mln0905

Produkt 1

HCID 86643317HCID 86643317, VerbindungAusbeute 92,6 %

Versuchsvorschrift

To a solution of 2-({5-[3-(Dimethylamino)propyl]-2-methylpyridin-3-yl}amino)-9-(trifluoromethyl)-5,7-dihydro-6H-pyrimido[5,4-d][1]benzazepine-6-thione (153 mg, 0.314 mmol) in Ethanol (5.1 mL, 87 mmol) under gentle reflux (oil bath at 85° C.) was added 0.89 M of Hydrochloric acid in Ethanol (7.0E2 μL, 0.63 mmol) (850 μl of conc. HCl in 10 ml of ethanol tritrated). The resulting solution was seeded and shortly thereafter solid formed. The mixture was allowed to cool at room temperature in the oil bath and was left overnight at room temperature. The solid was filtered off and dried under high vacuum to afford 2-({5-[3-(Dimethylamino)propyl]-2-methylpyridin-3-yl}amino)-9-(trifluoromethyl)-5,7-dihydro-6H-pyrimido[5,4-d][1]benzazepine-6-thione Dihydrochloride Salt as a yellow solid (163 mg, 92.6% yield).