Reaktionsgleichung
N[C:2]1[S:3][C:4]2[CH:10]=[CH:9][CH:8]=[C:7]([Cl:11])[C:5]=2[N:6]=1.N([O-])=O.[Na+].[BrH:16]>O.[Cu]Br>[Br:16][C:2]1[S:3][C:4]2[CH:10]=[CH:9][CH:8]=[C:7]([Cl:11])[C:5]=2[N:6]=1Komponenten
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 2
Reaktionsbedingungen
- Temperatur
- 0 °C
Versuchsvorschrift
Slurry 2-amino-4-chlorobenzothiazole (0.255 mol) in water (325 mL), heat to reflux and add 48% hydrobromic acid (130 mL). Maintain at reflux for 20 minutes, cool to 0° C. and add a solution of sodium nitrite (17.56 g, 0.255 mol) in water (90 mL), maintaining a temperature of 0° C. Stir at 0° C. for 15 minutes and add by dropwise addition (while keeping cold) to a rapidly stirring mixture of copper (I) bromide (42.03 g, 0.293 mol) in 48% hydrobromic acid (86 mL) and water (225 mL). Stir at room temperature for 20 minutes and then heat on a steam bath for an additional 20 minutes. Allow to stand overnight, extract into methylene chloride and dry (MgSO4). Evaporate the solvent in vacuo and purify by chromatography to give 2-bromo-4-chlorobenzothiazole.
Aufarbeitung
- temperatureto reflux
- temperatureMaintain
- temperatureat reflux for 20 minutes
- temperaturemaintaining a temperature of 0° C
- additionadd by dropwise addition (while keeping cold) to
- stirringa rapidly stirring
- stirringStir at room temperature for 20 minutes
- temperatureheat on a steam bath for an additional 20 minutes
- waitAllow to stand overnight
- extractionextract into methylene chloride
- dry with materialdry (MgSO4)
- customEvaporate the solvent in vacuo
- custompurify by chromatography
Quellen und Nachweise
- ORD-Eintrag
- ord-244dec9da798408c84c8871e7c369ede
- Quelldatensatz
- uspto-grants-1997_07
- Patentnummer
- US05650416
Verknüpfte Notizen
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