Synthesis and Characterization of Copper(I) Complex

This was synthesized following a modified literature procedure.^{28 (link)} Ph₂P(2-quinazoline) (123 mg, 0.4 mmol) and [Cu(MeCN)₄]PF₆ (97 mg, 0.26 mmol) were added to 1 dram vial. MeCN (1 ml) was added and the resulting yellow solution was stirred at r.t. (21 h), during which some product may form and give a yellow suspension. Further Et₂O may be added to precipitate more product. The precipitated solids were isolated via filtration and washed with Et₂O (5 ml) to give the crude product as a yellow powder that fluorescence orange (8.1 mg, 5.8 μmol, 11% yield). It may be further purified by redissolving it in minimal MeCN and precipitating with Et₂O twice.
δ_H (400 MHz, CDCl₃, ppm) 9.94 (br s), 8.29 (br s), 8.09 (t, J = 7.7 Hz), 7.94 (br s), 7.87 (t, J = 7.1 Hz), 7.16 (br s), 7.09 (br s).
δ_P{H} (162 MHz, CDCl₃, ppm): 10.68 (br s), −144.03 (sept, PF₆⁻).
δ_C (101 MHz, CDCl₃, ppm) 161.44, 149.10, 137.14, 133.14, 131.02, 130.80, 128.89, 128.22.
HRMS(ESI+): [C₂H₃CuN]⁺m/z = 103.9554, calcd = 103.9562. [C₆₀H₄₅CuN₆P₃]⁺m/z = 1005.2242, calcd = 1005.2215. [C₄₀H₃₀CuN₄P₂]⁺m/z = 691.1262, calcd = 691.1242. [C₂₂H₁₈CuN₃P]⁺m/z = 418.0545, calcd = 418.0534. [C₂₀H₁₅CuN₂P]⁺m/z = 377.0271, calcd = 377.0269.