Trivalent gold complexes and their application in photocatalytic reduction of water to hydrogen production
A technology for producing hydrogen from gold complexes and water, which is applied in organic compound/hydride/coordination complex catalysts, gold organic compounds, physical/chemical process catalysts, etc. It can solve the problems of poor ability to absorb visible light and slow catalytic rate
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Embodiment 1
[0032] 0.43mmol[Au(C^N^C)Cl] and 0.1ml phenylacetylene (molar ratio is 1:2) were dissolved in 20mg cuprous iodide, 35mL dichloromethane and 2mL triethylamine molar ratio: 1 :5460:14 in the mixed solution of composition, stirred at room temperature for 6h, after the reaction was finished, after the solvent was spin-dried, chromatographic separation was carried out in a silica gel column with a volume ratio of 2:1 n-hexane and dichloromethane as the eluent, The trivalent gold complex was obtained through the recrystallization process.
[0033] The trivalent gold complex is carried out nuclear magnetic resonance (H spectrogram sees figure 1 ), measured: 1 H NMR (DMSO, 500MHz): δ8.16 (1H, t, J = 8.0), 7.98 (2H, d, J = 8.0), 7.90 (4H, t, J = 6.0), 7.54 (2H, d, J =7.3), 7.41 (4H, m), 7.33 (3H, m). Elemental analysis, calculated value: C 25 h 16 NAu: C, 56.94; H, 3.06; N, 2.66. Calculated: C, 56.66; H, 3.07; N, 2.67. ESI-MS (Methanol): Found: 1076.83 [2×M+Na] + . Calculated valu...
Embodiment 2
[0035] Dissolve 0.52mmol [Au(C^N^C)Cl] and 0.79ml 3,6-di-tert-butyl-9-(4-ethynylphenyl)-9H-carbazole in a molar ratio of 2:3 in In the mixed solution that is made up of 20mg cuprous iodide, 35mL dichloromethane and 2mL triethylamine, stir 8h at room temperature, after the reaction finishes, after the solvent is spin-dried, in the silica gel column, be that the volume ratio is 2:1 n-hexane Chromatographic separation with dichloromethane as the eluent, and a trivalent gold complex is obtained through recrystallization.
[0036] The trivalent gold complex is carried out nuclear magnetic resonance (H spectrogram sees figure 2 ), measured: 1 H NMR (DMSO, 500MHz): δ8.31 (2H, s), 8.20 (1H, s), 7.99 (4H, t, J = 9.2), 7.94 (2H, s), 7.80 (2H, d, J = 7.6), 7.62 (2H, d, J=7.9), 7.52 (2H, d, J=7.9), 7.46 (2H, s), 7.38 (4H, m), 1.44 (16H, s). Elemental analysis, calculation Value: C 46 h 39 NAu: C, 68.74; H, 5.02; N, 1.74. Found: C, 68.48; H, 5.14; + . Calculated value: 804.77.
Embodiment 3
[0038] Mix 0.1mL phenylacetylene with 0.43mmol[Au(C^N^C)Cl], 0.38mmol[Au( t BuC^N^C t Bu)Cl] (molar ratio is 2:5) was added to the mixed solution consisting of 20mg cuprous iodide, 35mL dichloromethane and 2mL triethylamine, stirred at room temperature for 6h, after the reaction was finished, the solvent was spin-dried Chromatographic separation was carried out on a silica gel column with n-hexane and dichloromethane at a volume ratio of 2:1 as the eluent, and the trivalent gold complex was obtained through recrystallization.
[0039] The trivalent gold complex is carried out nuclear magnetic resonance (H spectrogram sees image 3 ), measured: 1 H NMR (DMSO, 500MHz): δ8.10 (1H, t, J = 8.0), 8.04 (2H, d, J = 1.5), 7.86 (2H, d, J = 8.0), 7.81 (2H, d, J =8.2), 7.49(2H, d, J=7.3), 7.42(2H, t, J=7.5), 7.35(3H, m), 1.34(18H, s). Elemental analysis, calculated value: C 33 h 32 NAu: C, 61.97; H, 5.04; N, 2.19. Found: C, 61.86; H, 5.12; + . Calculated value: 639.58.
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