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Potassium Carbonate → HCID 178501112, Verbindung

HRID 538054
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 538054
C([O-])([O-])=O.[K+].[K+].F[C:8]1[CH:13]=[C:12]([C:14]([F:17])([F:16])[F:15])[CH:11]=[CH:10][C:9]=1[N+:18]([O-:20])=[O:19].[CH3:21][O:22][C:23]([C@H:25]1[CH2:30][CH2:29][C@H:28]([CH2:31][NH2:32])[CH2:27][CH2:26]1)=[O:24]>CN(C=O)C>[CH3:21][O:22][C:23]([C@H:25]1[CH2:30][CH2:29][C@H:28]([CH2:31][NH:32][C:8]2[CH:13]=[C:12]([C:14]([F:17])([F:16])[F:15])[CH:11]=[CH:10][C:9]=2[N+:18]([O-:20])=[O:19])[CH2:27][CH2:26]1)=[O:24]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 37221693-fluoro-4-nitrobenzotrifluorideHCID 178501118HCID 178501118, Verbindung

Produkt 1

HCID 178501112HCID 178501112, VerbindungAusbeute 86,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

K2CO3 (1.6 g, 11.7 mmol), 2-Fluoro-1-nitro-4-trifluoromethyl-benzene (1.22 g, 5.8 mmol) and trans-4-Aminomethyl-cyclohexanecarboxylic acid methyl ester (1.00 g, 5.84 mmol) were dissolved in DMF (10 ml). The mixture was stirred at 50° C. overnight. The solvent was removed under reduced pressure and the crude product dissolved in DCM (15 ml) and washed with water (20 ml) and then with a solution of citric acid (1M, 5 ml). The organic solution was dried over Na2SO4, filtered and the solvent removed by evaporation to give solid material. This was washed with cyclohexane and then with isopropyl ether and purified by silica column using DCM/cyclo hexane (1:1) as eluent. 1.8 g (yield 86%) of the title compound were isolated.

Aufarbeitung

  1. customThe solvent was removed under reduced pressure
  2. dissolutionthe crude product dissolved in DCM (15 ml)
  3. washwashed with water (20 ml)
  4. dry with materialThe organic solution was dried over Na2SO4
  5. filtrationfiltered
  6. customthe solvent removed by evaporation
  7. customto give solid material
  8. washThis was washed with cyclohexane
  9. customwith isopropyl ether and purified by silica column

Quellen und Nachweise

ORD-Eintrag
ord-2d482fafe8e649b8841a8f7e5390fded
Quelldatensatz
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08865704B2

Notizen zur Reaktion

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