PALLADIUM PHTHALOCYANINE synthesis

Yield: 5.6 g

Reaction Conditions:

with palladium dichloride at 180; for 2 h;

Steps:

Synthesis of palladium(II) phthalocyanine
Palladium(II) phthalocyanine (PdPc) was synthesized by modifying slightly the procedure described for the synthesis of other metal phthalocyanines. A total of 5 g (0.039 mol) phthalonitrile and 1.77 g (0.01 mol) palladium chloride were mixed well and heated slowly under reflux to 140 °C while stirring over an oil bath, at which point the phthalonitrile melts and forms a brownish slurry. The reaction mixture was then heated to 180 °C and maintained at 180 °C for 2 h with constant stirring. The crude product was cooled to room temperature and the solid mass was finely ground and washed with methanol, hot alcohol and water to remove the intermediates and unreacted components. The product was dried in the oven for 1 h to obtain 5.6 g of a bluish green solid. Anal. for palladium(II) phthalocyanine, C₃₂H₁₆N₈Pd: Calc. (%) C, 62.09; H, 2.59; N, 18.11; Pd, 17.21. Found C, 61.73; H, 2.79; N, 18.45, Pd, 17.03. Electronic absorption, λ_max (nm): 328, 436, 617,661. IR absorption bands (cm^-1): 754(w), 871(s), 913(m), 950(w), 1069(w), 1093(m), 1114(s), 1164(s), 1287, 1326(s), 1361(m), 1415(w), 1463(m), 1504(w), 1556(s), 1605(w).

References:

Lokesh, Koodlur Sannegowda;Adriaens, Annemie [Dyes and Pigments,2013,vol. 96,# 1,p. 269 - 277]