Ruthenium polypyridine complex as well as preparation method and application thereof
A technology of ruthenium polypyridine and complexes, which is applied in the field of photoacid generators, and can solve the problems of large dosage of raw materials, large amount of raw materials, and low efficiency
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Embodiment 1
[0043] A ruthenium polypyridine complex of the formula,
[0044]
[0045] Its preparation comprises the following steps:
[0046] RuCl 3 ·xH 2 O (50mg, 0.19mmol) and 4,4'-dichloromethyl-2,2'-bipyridine (bcm-bpy) (152mg, 0.6mmol) in DMF solvent N 2 Reflux overnight under atmosphere and spin dry the solvent. Compound 3 was purified by silica gel column, the eluent was CH 3 CN / H 2 O / KNO 3 (10:4:1), the product was dissolved in water, and with NH 4 PF 6 Precipitate out. Refer to attached figure 1 and 2 . 1 H NMR (400MHz, CD 3 CN)δ8.49(s,6H),7.61(d,J=5.8Hz,6H),7.37(d,J=5.9Hz,6H),4.73(s,12H).HR ESI-MS:m / z =429.9834for(M-2PF 6 - ) 2+ .
[0047]The prepared above-mentioned ruthenium polypyridine complex was dissolved in water to a concentration of 10 μM, and irradiated with visible light with a wavelength of 520 nm, and the light intensity was 10 mW / cm 2 , the light time is 50s, and the photoacid efficiency is 50%. as attached image 3 It can be seen that the pH...
Embodiment 2
[0049] A ruthenium polypyridine complex of the formula,
[0050]
[0051] Its preparation comprises the following steps:
[0052] RuCl 3 ·xH 2 O (100mg, 0.38mmol) and LiCl (106mg), bpy (113mg, 0.8 mmol ) in DMF solvent N 2 Reflux overnight under atmosphere and spin dry the solvent. Add acetone to the obtained product, place it overnight in a refrigerator at 4°C, and filter to obtain a solid (intermediate, Ru(bpy) 2 Cl 2 ), 100mg Ru(bpy) 2 Cl 2 (0.19mmol) and bcm-bpy (50.6mg, 0.2 mmol ) in DMF solvent N 2 Reflux overnight under atmosphere and spin dry the solvent. Compound 1 was purified by silica gel column, the eluent was CH 3 CN / H 2 O / KNO 3 (10:4:1), the product was dissolved in water, and with NH 4 PF 6 sink out.
[0053] The prepared above-mentioned ruthenium polypyridine complex was dissolved in water to a concentration of 10 μM, and irradiated with visible light with a wavelength of 520 nm, and the light intensity was 10 mW / cm 2 , the light time is ...
Embodiment 3
[0055] A ruthenium polypyridine complex of the formula,
[0056]
[0057] Its preparation comprises the following steps:
[0058] RuCl 3 ·xH 2 O (100mg, 0.38mmol) and LiCl (106mg), bcm-bpy (204mg, 0.8mmol) in DMF solvent N 2 Reflux overnight under atmosphere and spin dry the solvent. Add acetone to the obtained product, place it overnight in a refrigerator at 4°C, and filter to obtain a solid (intermediate, Ru(bcm-bpy) 2 Cl 2 ), 100mg Ru(bcm-bpy) 2 Cl 2 (0.15mmol) and bpy (22.7mg, 0.16 mmol ) in DMF solvent N 2 Reflux overnight under atmosphere and spin dry the solvent. Compound 3 was purified by silica gel column, the eluent was CH 3 CN / H 2 O / KNO 3 (10:4:1), the product was dissolved in water, and with NH 4 PF 6 sink out.
[0059] The prepared above-mentioned ruthenium polypyridine complex was dissolved in water to a concentration of 10 μM, and irradiated with visible light with a wavelength of 520 nm, and the light intensity was 10 mW / cm 2 , the light tim...
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