Dinitrogen monophosphine compound and its preparation method and application, cuprous halide complex and its preparation method and application
A cuprous halide and complex technology, applied in the field of copper complexes, can solve the problems of low metal reserves, limited application, high price, etc.
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[0041] With [CuX(fpda)] 2 For example, fpda=2-[(2-dimethylamino-5-trifluoromethylphenyl)(phenyl)phosphino]-N,N-dimethyl-4-trifluoromethylaniline, X =I (complex 1), Br (complex 2) and Cl (complex 3).
[0042] The synthesis route of ligand fpda and copper (I) complex 1-3 is as follows. At 78°C, THF / Et 2 2-Dimethylamino-4- Trifluoromethylphenyllithium, and then add dichlorophenylphosphine to the mixture, after the reaction, separate and purify to obtain the ligand fpda with a yield of 44.1%. Then 1 equivalent of fpda ligand and 1 equivalent of CuX (X = I for 1, Br for 2, Cl for 3) in CH 3CN mixed, separated and purified to obtain complexes 1–3, with a yield of 80.0-83.4%. All Cu(I) complexes are air-stable and high-purity, soluble in common organic solvents such as dichloromethane, chloroform, acetonitrile, etc.
[0043]
Embodiment 1
[0045] Synthesis of ligand fpda: Add 1.6 g (6 mmol) of 2-bromo-N,N-dimethyl-5-trifluoromethylaniline to 30 mL of tetrahydrofuran / diethyl ether (1 / 1 v To the / v) solution, 2.5M 2.4 mL (6 mmol) of n-butyllithium in hexane was added dropwise. After the dropwise addition, continue to stir for 1h at the same temperature, then dropwise add 0.54g (3mmol) phenylphosphine dichloride thereto at the same temperature, after the dropwise addition, the reaction mixture appears light yellow, The solution was gradually warmed to room temperature and stirred overnight. Finally, 10 mL of deionized water was added to the reaction mixture to quench the reaction, and then the reaction mixture was extracted with dichloromethane. After several extractions, the organic phases were combined and dried with anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure to obtain The residue. The residue was separated and purified by silica gel column chromatography with petroleu...
Embodiment 2
[0047] Synthesis of complex 1: Add cuprous iodide (0.190g, 1.00mmol) to 30mL of CH dissolved in fpda (0.484g, 1.00mmol) 3 CN solution, the mixed solution was stirred in the dark at room temperature to form a green-yellow suspension, the reaction mixture was filtered, and the solvent was removed under reduced pressure to obtain a yellow powder, which was washed with CH 2 Cl 2 / CH 3 CN was recrystallized to give yellow-green crystals [CuI(fpda)] 2 0.563g, 83.4%. 1 H NMR (500MHz, CDCl 3 )δ: 7.75 7.68 (m, 4H), 7.56 (d, J=5Hz, 4H), 7.45-7.40 (m, 2H), 7.38 7.33 (m, 8H), 7.28 7.24 (m, 4H), 2.67 (s , 24H). 31 P NMR (200MHz, CDCl 3 ), δ=-26.34(s). Anal. Calcd for C 48 h 46 Cu 2 f 12 I 2 N 4 P 2 : C, 42.71; H, 3.44; N, 4.15. Found: C, 42.75; H, 3.46; N, 4.17. MS (MALDI-TOF): m / z calcd for [C 24 h 23 CuF 6 N 2 P] + , 547.0799. Found: 547.0827.
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