4,4'-Dimethyl-2,2'-bipyridine → 2-Pyridinecarboxylic acid, 4,5,6-trichloro-

Three 8 mL scintillation vials were charged with NiCl2.6H2O (12.0 mg, 0.051 mmol) and one of the following ligands: 6,6′-dimethyl-2,2′-bipyridyl, 4,4′-dimethyl-2,2′-bipyridyl or 5-methyl-1,10-phenanthroline (2:1 ligand/metal ratio). The vials were closed and purged with nitrogen for 5 min, after which the vials were charged with DMF (4.5 mL) and water (0.5 mL). The mixtures were allowed to stir for 5 min. To each of the vials was added zinc dust (0.22 g, 3.4 mmol), and the mixtures were allowed to stir under nitrogen for 35 min. Solid 3,4,5,6-tetrachloropicolinic acid (0.10 g, 0.4 mmol) was added to each through the top of the reactor. The reaction mixtures were allowed to stir at ambient temperature, 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.

1. customThe vials were closed
2. custompurged with nitrogen for 5 min
3. additionafter which the vials were charged with DMF (4.5 mL) and water (0.5 mL)
4. stirringto stir under nitrogen for 35 min
5. customThe reaction mixtures
6. stirringto stir at ambient temperature
7. customsamples were removed periodically
8. customreaction kinetics

ORD-Eintrag

ord-c09a4665212347838a50ee09399159d7

Quelldatensatz

uspto-grants-2016_09

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09440923B2