Hydrochloric Acid → (5-Fluoro-2-(1H-1,2,4-triazol-1-yl)phenyl)methanamine hydrochloride

HRID 1726582Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1726582
[F:1][C:2]1[CH:3]=[CH:4][C:5]([N:10]2[CH:14]=[N:13][CH:12]=[N:11]2)=[C:6]([CH:9]=1)[C:7]#[N:8].[ClH:15]>C(O)C>[ClH:15].[F:1][C:2]1[CH:3]=[CH:4][C:5]([N:10]2[CH:14]=[N:13][CH:12]=[N:11]2)=[C:6]([CH2:7][NH2:8])[CH:9]=1

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 218662545-fluoro-2-(1H-1,2,4-triazol-1-yl)benzonitrile

Produkt 1

HCID 21069930(5-Fluoro-2-(1H-1,2,4-triazol-1-yl)phenyl)methanamine hydrochlorideAusbeute 98 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A solution of intermediate 96, 5-fluoro-2-(1H-1,2,4-triazol-1-yl)benzonitrile (2.94 g, 15.59 mmol) in ethanol (100 mL) and 1N HCl (50 mL) was degassed by bubbling N2. Then, 10% Pd/C was added, the flask evacuated and vented to H2 three times and left on a Parr shaker under a H2 atmosphere (40 psi). After 6 h, the reaction mixture was filtered, concentrated and the aqueous solution lyophilized to afford the title compound (4.07 g, 98%) as a white powder. LCMS (M+H) calcd for C9H10FN4: 193.09; found: 193.15.

Aufarbeitung

  1. customby bubbling N2
  2. additionThen, 10% Pd/C was added
  3. customthe flask evacuated
  4. waitleft on a Parr shaker under a H2 atmosphere (40 psi)
  5. filtrationthe reaction mixture was filtered
  6. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-0b44c141e0164bb79f15fd1ea90bfb7c
Quelldatensatz
uspto-grants-2009_02
Patentnummer
US07491819B1

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