反応 #2161225

反応方程式

water

cobalt acetate tetrahydrate

porphyrin

( 2 )

tetrakis(4-ethynylphenyl)porphyrin

→

cobalt tetrakis(4-ethynylphenyl)porphyrin

収率 65.0%

溶媒

DMF

DMF

反応条件

後処理

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

実験手順

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.

出典