1-(4-Fluorophenyl)piperazine → 2-[3-[4-(4-fluorophenyl)-1-piperazinyl]propyl]-6,7-dimethyl-2H-1,4-benzothiazin-3(4H)-one
Reaktionsgleichung
Br[CH2:2][CH2:3][CH2:4][CH:5]1[C:10](=[O:11])[NH:9][C:8]2[CH:12]=[C:13]([CH3:17])[C:14]([CH3:16])=[CH:15][C:7]=2[S:6]1.[F:18][C:19]1[CH:24]=[CH:23][C:22]([N:25]2[CH2:30][CH2:29][NH:28][CH2:27][CH2:26]2)=[CH:21][CH:20]=1>C(OCC)(=O)C>[F:18][C:19]1[CH:20]=[CH:21][C:22]([N:25]2[CH2:30][CH2:29][N:28]([CH2:2][CH2:3][CH2:4][CH:5]3[C:10](=[O:11])[NH:9][C:8]4[CH:12]=[C:13]([CH3:17])[C:14]([CH3:16])=[CH:15][C:7]=4[S:6]3)[CH2:27][CH2:26]2)=[CH:23][CH:24]=1Komponenten
4
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 110 °C
Versuchsvorschrift
In 10 ml of ethyl acetate were dissolved 628 mg of 2-(3-bromopropyl)-6,7-dimethyl-2H-1,4-benzothiazin-3(4H)-one and 721 mg of 1-(4-fluorophenyl)piperazine. The solution was concentrated and the concentrate was stirred at 110° C. for one hour, diluted with water, and extracted with ethyl acetate. The ethyl acetate layer was washed with water, dried over MgSO4 and concentrated to give 2-[3-[4-(4-fluorophenyl)-1-piperazinyl]propyl]-6,7-dimethyl-2H-1,4-benzothiazin-3(4H)-one (650 mg, 78.6%). Recrystallization from methanol gave colorless prisms, m.p. 161°-162° C.
Aufarbeitung
- concentrationThe solution was concentrated
- additiondiluted with water
- extractionextracted with ethyl acetate
- washThe ethyl acetate layer was washed with water
- dry with materialdried over MgSO4
- concentrationconcentrated
Quellen und Nachweise
- ORD-Eintrag
- ord-00d3682dc3a84113a1e9543fe0a112b5
- Quelldatensatz
- uspto-grants-1987_02
- Patentnummer
- US04640916
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