Reaktion #2161225

Reaktionsgleichung

water

cobalt acetate tetrahydrate

porphyrin

( 2 )

tetrakis(4-ethynylphenyl)porphyrin

→

cobalt tetrakis(4-ethynylphenyl)porphyrin

Ausbeute 65.0%

Lösungsmittel

DMF

DMF

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe mixture obtained
2. 2
   Temperaturwas refluxed for 20 hours
3. 3
   ExtraktionThe mixture was subsequently extracted with ethanol (4×200 ml)
4. 4
   Sonstigethe organic phase was then evaporated
5. 5
   workup.DISSOLUTIONThe residue was dissolved in 300 ml of ethanol
6. 6
   Waschenthe organic phase was washed with 3×200 ml of water
7. 7
   Trocknendried over sodium sulfate
8. 8
   SonstigeThe solvent was evaporated off

Vorschrift

A solution of 8.71 g (35 mmol) of cobalt acetate tetrahydrate (Co(CH3COO)2.4H2O) in 100 ml of DMF was added portionwise to a solution of 1.7 g (2.39 mmol) of porphyrin TEPP (2) as obtained above in step 2), in 500 ml of DMF. The mixture obtained was refluxed for 20 hours. The heating was stopped and 150 ml of water were added to the reaction medium. The mixture was subsequently extracted with ethanol (4×200 ml) and the organic phase was then evaporated. The residue was dissolved in 300 ml of ethanol, and the organic phase was washed with 3×200 ml of water and dried over sodium sulfate. The solvent was evaporated off and the cobalt tetrakis(4-ethynylphenyl)porphyrin (Co-TEPP) (4) (1.19 g; 1.55 mmol; yield: 65%) was obtained in the form of a powder that was purple/black in color, and red in solution in chloroform.

Quelle