Synthesis
2.1.4.1 Synthesis of cis-dichloro(1,5-cyclooctadiene)platinum(II), [Pt(cod)Cl2] (0014): K2PtCl4 (1.000 g, 2.4 mmol) was dissolved in water (16 mL) and the resulting solution was filtered. Acetic acid (24 mL) and 1,5-cyclooctadiene (cod) (1.00 mL, 8.1 mmol) were sequentially added to the filtrate under light protection. The reaction mixture was stirred and heated in a water bath at about 100°C. Within 30 minutes, the dark red solution gradually changed to a pale yellow color with the formation of a precipitate. After about 2 h, the solution was concentrated to a volume of 10 mL by distillation under reduced pressure, after which the resulting precipitate was separated by centrifugation and washed sequentially with water, ethanol and ether. Product yield: 703 mg (80%).1H NMR (CDCl3) δ: 5.60 (4H, t, CH), 2.70 (2H, m, CH2-CH), 2.30-2.16 (2H, m, CH2-CH) ppm; 13C{1H} NMR (CDCl3) δ: 100.0 (CH), 30.0 (CH2) ppm. 195Pt NMR (CDCl3) δ: -3340 ppm.
References
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