반응 #2161225

반응 방정식

water

cobalt acetate tetrahydrate

porphyrin

( 2 )

tetrakis(4-ethynylphenyl)porphyrin

→

cobalt tetrakis(4-ethynylphenyl)porphyrin

수율 65.0%

용매

DMF

DMF

반응 조건

후처리

1. 1
   기타The mixture obtained
2. 2
   온도was refluxed for 20 hours
3. 3
   추출The mixture was subsequently extracted with ethanol (4×200 ml)
4. 4
   기타the organic phase was then evaporated
5. 5
   workup.DISSOLUTIONThe residue was dissolved in 300 ml of ethanol
6. 6
   세척the organic phase was washed with 3×200 ml of water
7. 7
   건조dried over sodium sulfate
8. 8
   기타The solvent was evaporated off

실험 절차

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.

출처