Pyridine-2-carbonitrile → HCID 59750419, Verbindung

HRID 499273Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 499273
[F:1][C:2]1[C:7]([C:8]([OH:10])=O)=[C:6]([SH:11])[CH:5]=[CH:4][CH:3]=1.[C:12]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][N:15]=1)#[N:13]>N1C=CC=CC=1>[F:1][C:2]1[C:7]2[C:8](=[O:10])[N:13]=[C:12]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][N:15]=3)[S:11][C:6]=2[CH:5]=[CH:4][CH:3]=1

Komponenten

4

Edukt 2

HCID 7522Pyridine-2-carbonitrileHCID 229394662-Fluoro-6-sulfanylbenzoic acid

Produkt 1

HCID 59750419HCID 59750419, VerbindungAusbeute 1,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Reaktionsbedingungen

Temperatur
135 °C

Versuchsvorschrift

A mixture of 6-fluoro-2-mercaptobenzoic acid (5.00 g, 29.0 mmol), 2-cyanopyridine (3.05 g, 29.3 mmol) and pyridine (30.0 ml) was refluxed at 135° C. for 48 hrs as described in Example 9. The reaction mixture was concentrated. The residue was subjected to a silica gel column chromatography and eluted with hexane-ethyl acetate (2:1, v/v). The resultant product was recrystallized from ethanol to give the titled compound (0.11 g, 1%).

Aufarbeitung

  1. concentrationThe reaction mixture was concentrated
  2. washeluted with hexane-ethyl acetate (2:1
  3. customThe resultant product was recrystallized from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-2d08b992986c4d38bc74b6e9153279d5
Quelldatensatz
uspto-grants-2010_08
Patentnummer
US07767665B2

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