Cesium carbonate → HCID 24822778, Verbindung

HRID 1925363Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1925363
[F:1][C:2]1[C:11]([OH:12])=[CH:10][CH:9]=[C:8]2[C:3]=1[CH:4]=[CH:5][CH:6]=[C:7]2[C:13]([OH:15])=[O:14].C([O-])([O-])=O.[Cs+].[Cs+].Cl[C:23]1[C:32]2[C:27](=[CH:28][C:29]([O:35][CH3:36])=[C:30]([O:33][CH3:34])[CH:31]=2)[N:26]=[CH:25][CH:24]=1>CS(C)=O>[CH3:34][O:33][C:30]1[CH:31]=[C:32]2[C:27](=[CH:28][C:29]=1[O:35][CH3:36])[N:26]=[CH:25][CH:24]=[C:23]2[O:12][C:11]1[C:2]([F:1])=[C:3]2[C:8](=[CH:9][CH:10]=1)[C:7]([C:13]([OH:15])=[O:14])=[CH:6][CH:5]=[CH:4]2

Komponenten

5

Edukt 3

HCID 10796Cesium carbonateHCID 4596104-Chloro-6,7-dimethoxyquinolineHCID 248246045-Fluoro-6-hydroxynaphthalene-1-carboxylic acid

Produkt 1

HCID 24822778HCID 24822778, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 679Dimethyl SulfoxideLösungsmittel

Versuchsvorschrift

To a solution of 5-fluoro-6-hydroxy-1-naphthoic acid (1 g, 4.87 mmol) in DMSO (5 mL), Cs2CO3 (4.75 g, 14.61 mmol) was added in one portion. The mixture was stirred at RT 10 min. To the suspension, 4-chloro-6,7-dimethoxyquinoline (1.09 g, 4.87 mmol) was added and the mixture heated to 140° C. O/N. The mixture was allowed to cool to RT, pH adjusted to 7 and the resulting solid filtered and rinsed with water. The title compound was obtained as a tan solid.

Aufarbeitung

  1. temperaturethe mixture heated to 140° C
  2. temperatureto cool to RT
  3. filtrationthe resulting solid filtered
  4. washrinsed with water

Quellen und Nachweise

ORD-Eintrag
ord-1cd174abc31e4697a268cfdd4bc1a4c5
Quelldatensatz
uspto-grants-2012_05
Patentnummer
US08178557B2

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