反应 #2161225

反应方程式

water

cobalt acetate tetrahydrate

porphyrin

( 2 )

tetrakis(4-ethynylphenyl)porphyrin

→

cobalt tetrakis(4-ethynylphenyl)porphyrin

收率 65.0%

溶剂

DMF

DMF

反应条件

后处理

1. 1
   其他The mixture obtained
2. 2
   温度was refluxed for 20 hours
3. 3
   萃取The mixture was subsequently extracted with ethanol (4×200 ml)
4. 4
   其他the organic phase was then evaporated
5. 5
   workup.DISSOLUTIONThe residue was dissolved in 300 ml of ethanol
6. 6
   洗涤the organic phase was washed with 3×200 ml of water
7. 7
   干燥dried over sodium sulfate
8. 8
   其他The solvent was evaporated off

实验过程

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.

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