Potassium Carbonate → HCID 86683431, Verbindung
Reaktionsgleichung
Br[C:2]1[S:3][C:4]2[CH:10]=[C:9]([OH:11])[CH:8]=[CH:7][C:5]=2[N:6]=1.Cl.[CH:13]([N:16]1[CH2:21][CH2:20][NH:19][CH2:18][CH2:17]1)([CH3:15])[CH3:14].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[CH:13]([N:16]1[CH2:21][CH2:20][N:19]([C:2]2[S:3][C:4]3[CH:10]=[C:9]([OH:11])[CH:8]=[CH:7][C:5]=3[N:6]=2)[CH2:18][CH2:17]1)([CH3:15])[CH3:14]Komponenten
5
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 100 °C
Versuchsvorschrift
2-Bromo-6-hydroxybenzothiazole (345 mg, 1.5 mmol), 1-isopropyl-piperazine hydrochloride (271 mg, 1.65 mmol) and dry potassium carbonate (828 mg, 6.00 mmol), were dissolved in 6 mL, of dry N,N-dimethylformamide. The resulted pale brown solution was stirred at 100° C. for 18 h in a closed vial. The reaction mixture was evaporated, suspended in 20 mL of water and extracted with dichloromethane (3×15 mL). The combined organic layers were washed with saturated sodium bicarbonate and brine, then dried over MgSO4. After evaporation the residue was purified by column chromatography (Kieselgel 60) using chloroform-methanol 49:1 as the eluent. The title compound (76 mg, 0.27 mmol, 18%) was obtained as a white solid.
Aufarbeitung
- customThe reaction mixture was evaporated
- extractionextracted with dichloromethane (3×15 mL)
- washThe combined organic layers were washed with saturated sodium bicarbonate and brine
- dry with materialdried over MgSO4
- customAfter evaporation the residue
- customwas purified by column chromatography (Kieselgel 60)
Quellen und Nachweise
- ORD-Eintrag
- ord-e67e41a5abab4f0da95fb83afa0fbbd4
- Quelldatensatz
- uspto-grants-2015_05
- Patentnummer
- US09040714B2
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