Benzyl Bromide → HCID 21891956, Verbindung

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Reaktionsgleichung

C(=O)([O-])[O-].[K+].[K+].[Cl:7][C:8]1[C:17]([CH:18]=[O:19])=[CH:16][C:15]2[C:10](=[CH:11][C:12]([F:21])=[C:13]([OH:20])[CH:14]=2)[N:9]=1.[CH2:22](Br)[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1>CN(C)C=O>[CH2:22]([O:20][C:13]1[CH:14]=[C:15]2[C:10](=[CH:11][C:12]=1[F:21])[N:9]=[C:8]([Cl:7])[C:17]([CH:18]=[O:19])=[CH:16]2)[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1

Komponenten

Reaktionsbedingungen

Temperatur: 0 °C

Versuchsvorschrift

Potassium carbonate (9.2 g, 66 mmol) is added to a solution of 2-chloro-7-fluoro-6-hydoxy-3-quinolinecarbaldehyde (obtained according to 1.c, 13 g, 58 mmol) in anhydrous N,N-dimethylformamide (120 ml) and the mixture, placed under an argon atmosphere, is cooled down to 0° C. Benzyl bromide (7.9 ml, 66 mmol) is added dropwise and the reaction medium is maintained under agitation at ambient temperature for 16 hours. The reaction medium is then poured into ice cold water (200 ml) and the resulting yellow solid is filtered, then taken up in ethanol (200 ml) and concentrated under reduced pressure. The residue is taken up in ethyl ether (200 ml) and the resulting yellow solid is filtered then dried under reduced pressure in order to produce 15 g (82%) of a yellow solid, m.p. 228° C.

Aufarbeitung

temperaturethe reaction medium is maintained under agitation at ambient temperature for 16 hours
filtrationthe resulting yellow solid is filtered
concentrationconcentrated under reduced pressure
filtrationthe resulting yellow solid is filtered
customthen dried under reduced pressure in order

Quellen und Nachweise

ORD-Eintrag: ord-e1c5daaabefb431ea5f0d8310e37535d
Quelldatensatz: uspto-grants-2002_08
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US06436951B1

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