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Triphenylphosphine → HCID 59321464, Verbindung

HRID 2423510
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2423510
Br[C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]=[C:7]([C:12]([O:14][CH2:15][CH3:16])=[O:13])[CH:6]=[CH:5]2.[OH:17][C:18]1[CH:23]=[CH:22][C:21](B(O)O)=[CH:20][C:19]=1[CH3:27].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.P([O-])([O-])([O-])=O.[K+].[K+].[K+]>C([O-])(=O)C.[Pd+2].C([O-])(=O)C.C(OCC)(=O)C.O.O1CCOCC1>[OH:17][C:18]1[CH:23]=[CH:22][C:21]([C:2]2[CH:3]=[C:4]3[C:9](=[CH:10][CH:11]=2)[N:8]=[C:7]([C:12]([O:14][CH2:15][CH3:16])=[O:13])[CH:6]=[CH:5]3)=[CH:20][C:19]=1[CH3:27]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

9

Edukt 4

HCID 11776TriphenylphosphineHCID 62657Potassium Phosphate, TribasicHCID 45082971(4-Hydroxy-3-methylphenyl)boronic acidHCID 53404703Ethyl 6-bromoquinoline-2-carboxylate

Produkt 1

HCID 59321464HCID 59321464, VerbindungAusbeute 40 %

Reagenzien, Katalysatoren, Lösungsmittel 4

HCID 167845
palladium(II) acetate
Katalysator
HCID 962WaterLösungsmittel2×
HCID 8857Ethyl AcetateLösungsmittel
HCID 312751,4-DioxaneLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

Palladium(II)acetate (4.7 mg, 21.0 μmol) was added to ethyl 6-bromo-2-quinolinecarboxylate (117.8 mg, 420.5 μmol), (4-hydroxy-3-methylphenyl)boronic acid (95.9 mg, 630.8 μmol), triphenylphosphine (11.0 mg, 42.1 μmol), and potassium phosphate (312.4 mg, 1.47 mmol). Then, dioxane (4.2 mL) was added to the mixture, followed by water (42 μL), and the reaction mixture was heated open to the atmosphere at 60° C. in an oil bath for 16 hours, then allowed to cool to room temperature. Water was added, followed by ethyl acetate, and the mixture was filtered through Celite®. The filtrate was extracted with ethyl acetate, and the organic layer was dried over anhydrous magnesium sulfate, then filtered and concentrated. The residue was purified by silica gel chromatography eluting with 2:3 ethyl acetate:hexanes to give 51.4 mg (40%) of ethyl 6-(4-hydroxy-3-methylphenyl)-2-quinolinecarboxylate as a solid. 1H NMR (400 MHz, d6-DMSO): δ 9.64 (s, 1H), 8.55 (d, J=9 Hz, 1H), 8.27 (s, 1H), 8.18-8.13 (m, 2H), 8.11 (d, J=8 Hz, 1H), 7.62 (s, 1H), 7.53 (dd, J=8, 2 Hz, 1H), 6.91 (d, J=8 Hz, 1H), 4.42 (q, J=7 Hz, 2H), 2.22 (s, 3H), 1.38 (t, J=7 Hz, 3H). ESI-LCMS m/z 308 (M+H)+.

Aufarbeitung

  1. temperatureto cool to room temperature
  2. filtrationthe mixture was filtered through Celite®
  3. extractionThe filtrate was extracted with ethyl acetate
  4. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe residue was purified by silica gel chromatography
  8. washeluting with 2:3 ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-6c01c69632f6478c92bd1f509e6a6100
Quelldatensatz
uspto-grants-2011_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07960552B2

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