2,2'-Bipyridine → 2-Pyridinecarboxylic acid, 4,5,6-trichloro-

HRID 59597

Reaktionsgleichung

Reaktionsgleichung von HRID 59597
N1C=CC=CC=1C1C=CC=CN=1.Cl[C:14]1[C:15]([C:23]([OH:25])=[O:24])=[N:16][C:17]([Cl:22])=[C:18]([Cl:21])[C:19]=1[Cl:20]>[Zn].C(#N)C>[Cl:20][C:19]1[C:18]([Cl:21])=[C:17]([Cl:22])[N:16]=[C:15]([C:23]([OH:25])=[O:24])[CH:14]=1

Komponenten

5

Edukt 2

HCID 14742,2'-BipyridineHCID 826463,4,5,6-Tetrachloropyridine-2-carboxylic acid

Produkt 1

HCID 129936922-Pyridinecarboxylic acid, 4,5,6-trichloro-

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23994ZincKatalysatorHCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

An 8 mL scintillation vial was charged with NiCl2.6H2O (12.5 mg, 0.053 mmol) and 2,2′-bipyridine (18.2 mg, 0.117 mmol). The vial was closed and purged with nitrogen for 5 min, after which the vial was charged with DMF (4.5 mL) and methyl alcohol (CH3OH; 0.5 mL). The mixture was allowed to stir for 5 min. To the vial was added zinc dust (0.225 g, 3.4 mmol), and the mixture was allowed to stir under nitrogen for 35 min. Solid 3,4,5,6-tetrachloropicolinic acid (0.110 g, 0.4 mmol) was added through the top of the reactor. The reaction mixture was allowed to stir at 14° C. and samples were removed periodically to determine reaction kinetics. The samples (˜0.01 mL of reaction mixture diluted to 1.5 mL with acetonitrile) were analyzed by a calibrated HPLC method.

Aufarbeitung

  1. customThe vial was closed
  2. custompurged with nitrogen for 5 min
  3. additionafter which the vial was charged with DMF (4.5 mL) and methyl alcohol (CH3OH; 0.5 mL)
  4. stirringto stir under nitrogen for 35 min
  5. stirringto stir at 14° C.
  6. customsamples were removed periodically
  7. customreaction kinetics

Quellen und Nachweise

ORD-Eintrag
ord-6ca30213f04a49b687f25abc4afd206f
Quelldatensatz
uspto-grants-2016_09
Patentnummer
US09440923B2

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