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Benzylamine → N-benzyl-3,5,6-trifluoropyridin-2-amine

HRID 1274662
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1274662
F[C:2]1[C:7]([F:8])=[CH:6][C:5]([F:9])=[C:4]([F:10])[N:3]=1.[CH2:11]([NH2:18])[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1>C(#N)C>[CH2:11]([NH:18][C:2]1[C:7]([F:8])=[CH:6][C:5]([F:9])=[C:4]([F:10])[N:3]=1)[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1
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Komponenten

4

Edukt 2

HCID 7504BenzylamineHCID 1377492,3,5,6-Tetrafluoropyridine

Produkt 1

HCID 22121263N-benzyl-3,5,6-trifluoropyridin-2-amineAusbeute 84,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

To 50 ml of acetonitrile were added 12.0 g of 2,3,5,6-tetrafluoropyridine and 18.0 g of benzylamine, and the mixture was stirred under reflux condition for 2 hours, and the solvent and the like were distilled off. To the residue was added 150 ml of ethyl acetate, and the mixture was washed twice with 150 ml of distilled water and 150 ml of 10% aqueous solution of citric acid. The ethyl acetate layer was dried over anhydrous magnesium sulfate and concentrated under reduced pressure to obtain 16.0 g of the title compound as a pale yellow oil.

Aufarbeitung

  1. temperatureunder reflux condition for 2 hours
  2. distillationthe solvent and the like were distilled off
  3. additionTo the residue was added 150 ml of ethyl acetate
  4. washthe mixture was washed twice with 150 ml of distilled water and 150 ml of 10% aqueous solution of citric acid
  5. dry with materialThe ethyl acetate layer was dried over anhydrous magnesium sulfate
  6. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-4f7edaf7fa4e46d4b84306668461a03e
Quelldatensatz
uspto-grants-2000_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06156903

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