Hydrochloric Acid → HCID 23358997, Verbindung
Reaktionsgleichung
S(=O)(=O)(O)O.N([O-])=O.[Na+].[F:10][C:11]1[C:17]([F:18])=[C:16]([CH3:19])[C:15]([F:20])=[CH:14][C:12]=1N.[ClH:21]>C(O)(=O)C.[Cu]Cl>[F:18][C:17]1[C:11]([F:10])=[C:12]([Cl:21])[CH:14]=[C:15]([F:20])[C:16]=1[CH3:19]Komponenten
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 2
Reaktionsbedingungen
- Temperatur
- 70 °C
Versuchsvorschrift
To conc. sulfuric acid (3 ml) is added sodium nitrite (0.3 g). The mixture is stirred at 70° C. for 10 minutes and then cooled to below 40° C. and thereto a solution of 2,3,5-trifluoro-4-methylaniline (0.48 g) in acetic acid (5 ml) is added dropwise below 40° C. After stirring for 30 minutes, the reaction mixture is added dropwise to a solution of copper (I) chloride (1.04 g) in conc. hydrochloric acid (10.4 ml) and the mixture is stirred at 80° C. for 30 minutes and then cooled. The resultant mixture is poured into ice-water, extracted with dichloromethane, and the extract is washed with water and dried. The solvent is distilled off under reduced pressure and purified by silica-gel column-chromatography (eluent; dichloromethane: n-hexane=1:4) to give 2,3,6-trifluoro-4-chlorotoluene (0.22 g).
Aufarbeitung
- temperaturecooled to below 40° C.
- stirringAfter stirring for 30 minutes
- stirringthe mixture is stirred at 80° C. for 30 minutes
- temperaturecooled
- extractionextracted with dichloromethane
- washthe extract is washed with water
- customdried
- distillationThe solvent is distilled off under reduced pressure
- custompurified by silica-gel column-chromatography (eluent; dichloromethane: n-hexane=1:4)
Quellen und Nachweise
- ORD-Eintrag
- ord-9eea9288c44845239e59941f5d1a9cf0
- Quelldatensatz
- uspto-grants-1997_01
- Patentnummer
- US05591744
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