Reacción #87875

Ecuación de reacción

2,2′-bipyridine

3,4,5,6-tetrachloropicolinic acid

→

4,5,6-trichloropicolinic Acid

Disolventes

acetonitrile

Condiciones de reacción

Tratamiento posterior

1. 1
   OtroThe vial was closed
2. 2
   Otropurged with nitrogen for 5 min
3. 3
   workup.ADDITIONafter which the vial was charged with DMF (4.5 mL) and methyl alcohol (CH3OH; 0.5 mL)
4. 4
   workup.STIRRINGto stir under nitrogen for 35 min
5. 5
   workup.STIRRINGto stir at 14° C.
6. 6
   Otrosamples were removed periodically
7. 7
   Otroreaction kinetics

Procedimiento

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.

Fuente