Sodium Iodide → HCID 57917660, Verbindung

HRID 1878433Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1878433
Cl[CH2:2][C:3]1[CH:4]=[C:5]([CH:15]=[CH:16][CH:17]=1)[C:6]([NH:8][CH:9]1[CH2:12][C:11]([F:14])([F:13])[CH2:10]1)=[O:7].[N:18]1([C:24]([O:26][C:27]([CH3:30])([CH3:29])[CH3:28])=[O:25])[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]1.C(=O)([O-])[O-].[K+].[K+].[I-].[Na+]>C(#N)C>[F:13][C:11]1([F:14])[CH2:12][CH:9]([NH:8][C:6]([C:5]2[CH:4]=[C:3]([CH:17]=[CH:16][CH:15]=2)[CH2:2][N:21]2[CH2:20][CH2:19][N:18]([C:24]([O:26][C:27]([CH3:30])([CH3:29])[CH3:28])=[O:25])[CH2:23][CH2:22]2)=[O:7])[CH2:10]1

Komponenten

6

Edukt 4

HCID 5238Sodium IodideHCID 11430Potassium CarbonateHCID 143452tert-Butyl piperazine-1-carboxylateHCID 668783523-(chloromethyl)-N-(3,3-difluorocyclobutyl)benzamide

Produkt 1

HCID 57917660HCID 57917660, VerbindungAusbeute 98,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

3-(Chloromethyl)-N-(3,3-difluorocyclobutyl)benzamide (12.82 mmol, 3.33 g), tert-butyl piperazine-1-carboxylate (12.82 mmol, 2.388 g), potassium carbonate (38.5 mmol, 5.32 g) and sodium iodide (2.56 mmol, 0.384 g) were combined and heated at reflux in acetonitrile (50 ml) for 2 hours. The solvent was removed under reduced pressure and the residue taken up in dichloromethane, washed with water, dried over sodium sulfate and concentrated under vacuum to afford the title compound (5.179 g).

Aufarbeitung

  1. temperatureheated
  2. customThe solvent was removed under reduced pressure
  3. washwashed with water
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-97e3627ab6f8437cb5236f74099bc6a5
Quelldatensatz
uspto-grants-2012_11
Patentnummer
US08314091B2

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