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ChemicalBook CAS DataBase List COBALT TPP
14172-90-8

COBALT TPP synthesis

5synthesis methods
-

Yield:14172-90-8 93%

Reaction Conditions:

with sodium acetate;potassium carbonate in N,N-dimethyl-formamide;chlorobenzene at 150;

Steps:

4.4 General procedure for M(TPP)
General procedure: In a 250mL distillation flask, 5,10,15,20-tetraphenylporphyrin (H2TPP) (0.50g, 0.81mmol) and NaOAc (0.30g, 3.6mmol) was stirred in 75mL of chlorobenzene and 50mL of DMF. After the addition of two equivalents of metal acetate, a Soxhlet extractor with a cellulose filter thimble filled with ~3g of K2CO3 was attached to the distillation flask. The assembly was completed with a condenser on the top of the extractor; and then the mixture was heated to reflux at 150°C overnight. The reaction extent was monitored by TLC or UV-Vis until all the H2TPP was consumed. After the reaction was compete, the solvent was removed under vacuum. The remaining solid was dissolved in 150mL of chloroform, and washed with water (50mL×3). The organic layer was further washed with a saturated sodium bicarbonate solution (50mL×3), and then dried over K2SO4. After removal of the solvent in vacuo, the solid was recrystallized from chloroform/heptane.

References:

Yao, Shu A.;Hansen, Christopher B.;Berry, John F. [Polyhedron,2013,vol. 58,p. 2 - 6]

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