Potassium Carbonate → HCID 86670946, Verbindung

HRID 515303Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 515303
Cl[C:2]1[C:3]([CH2:10][CH:11]2[CH2:16][CH2:15][NH:14][CH2:13][CH2:12]2)=[CH:4][C:5]([F:9])=[C:6]([CH:8]=1)[NH2:7].Br[CH2:18][C:19]1[CH:24]=[CH:23][C:22]([C:25]([OH:34])([C:30]([F:33])([F:32])[F:31])[C:26]([F:29])([F:28])[F:27])=[CH:21][CH:20]=1.C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[NH2:7][C:6]1[CH:8]=[CH:2][C:3]([CH2:10][CH:11]2[CH2:16][CH2:15][N:14]([CH2:18][C:19]3[CH:20]=[CH:21][C:22]([C:25]([OH:34])([C:26]([F:27])([F:28])[F:29])[C:30]([F:31])([F:32])[F:33])=[CH:23][CH:24]=3)[CH2:13][CH2:12]2)=[CH:4][C:5]=1[F:9]

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 235273962-[4-(Bromomethyl)phenyl]-1,1,1,3,3,3-hexafluoropropan-2-olHCID 67192724HCID 67192724, Verbindung

Produkt 1

HCID 86670946HCID 86670946, VerbindungAusbeute 99,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

5-Chloro-2-fluoro-4-(piperidin-4-ylmethyl)aniline (1.730 mmol, 420 mg), 2-(4-(bromomethyl)phenyl)-1,1,1,3,3,3-hexafluoropropan-2-ol (1.730 mmol, 583 mg) and potassium carbonate (3.46 mmol, 478 mg) were combined and stirred at room temperature in acetonitrile (20 mL) for 2 hours. The reaction mixture was filtered and the filtrate concentrated under vacuum. The residue was purified by SCX chromatography to afford the title compound (800 mg). MS (ESI) m/z 499.5 [M+H]+

Aufarbeitung

  1. filtrationThe reaction mixture was filtered
  2. concentrationthe filtrate concentrated under vacuum
  3. customThe residue was purified by SCX chromatography

Quellen und Nachweise

ORD-Eintrag
ord-0dae16f0457f421ba163afb183d1f812
Quelldatensatz
uspto-grants-2015_08
Patentnummer
US09108939B2

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