Microwave-assisted preparation of polypyridine ruthenium(ii) complexes
A microwave-assisted, complex technology, applied in the field of compounds, achieves the effects of high yield, improved reaction conversion, and rapid synthesis
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Embodiment 1
[0021] Example 1 Preparation of polypyridine ruthenium (II) complexes (1)
[0022] 1. Preparation of (1,8-dihydroxy-9,10-anthraquinone)imidazo[4,5-f][1,10]phenanthroline (HAIP)
[0023] Add to a 30 mL microwave Pyrex reaction tube: o-phenanthroline 5,6-dione (0.315 g, 1.50 mmol), 1,8-dihydroxy-9,10-anthraquinone-3-aldehyde (603.0 mg, 2.25 mmol), ammonium acetate 4.5 g and glacial acetic acid 20 mL. Microwave was irradiated at 100°C for 20 min. After the reaction, the reaction solution was poured into 27 mL of distilled water, and the pH value was adjusted to 7 with concentrated ammonia water, resulting in a large amount of precipitation. Filter and dry to obtain a yellow crude product, which is purified by a 60-80 mesh silica gel column with absolute ethanol as the eluent, and the yield is 89.5%. ESI-MS: 459.4 (M+H).
[0024] 、Cis-[Ru(bpy) 2 (Cl) 2 ]·2H 2 O synthesis
[0025] In a 50 mL three-neck flask, add: bipyridine (1.87 g, 12 mmol), lithium chloride (2.43 g, 57.6 ...
Embodiment 2
[0032] Example 2 Preparation of polypyridine ruthenium (II) complexes (two)
[0033] 1. Preparation of HAIP
[0034] Add to a 30 mL microwave Pyrex reaction tube: o-phenanthroline 5,6-dione (0.315 g, 1.50 mmol), 1,8-dihydroxy-9,10-anthraquinone-3-aldehyde (603.0 mg, 2.25 mmol), ammonium acetate 4.5 g and glacial acetic acid 20 mL. Microwave was irradiated at 80°C for 60 min. After the reaction, the reaction solution was poured into 27 mL of distilled water, and the pH value was adjusted to 7 with concentrated ammonia water, resulting in a large amount of precipitation. Filter and dry to obtain a yellow crude product, which is purified by a 60-80 mesh silica gel column with absolute ethanol as the eluent, and the yield is 84%. ESI-MS: 459.4 (M+H).
[0035] 、Cis-[Ru(bpy) 2 (Cl) 2 ]·2H 2 O synthesis
[0036] With embodiment 1.
[0037] 、Cis-[Ru(phen) 2 (Cl) 2 ]·2H 2 O synthesis
[0038] With embodiment 1.
[0039] 、[Ru(bpy) 2 HAIP]·(PF 6 ) 2 preparation of
[004...
Embodiment 3
[0043] Example 3 Preparation of Polypyridine Ruthenium (II) Complexes (3)
[0044] 1. Preparation of HAIP
[0045] Add to a 30 mL microwave Pyrex reaction tube: o-phenanthroline 5,6-dione (0.315 g, 1.50 mmol), 1,8-dihydroxy-9,10-anthraquinone-3-aldehyde (603.0 mg, 2.25 mmol), ammonium acetate 4.5 g and glacial acetic acid 20 mL. Microwave was irradiated at 200°C for 10 min. After the reaction, the reaction solution was poured into 27 mL of distilled water, and the pH value was adjusted to 7 with concentrated ammonia water, resulting in a large amount of precipitation. Filter and dry to obtain a yellow crude product, which is purified by a 60-80 mesh silica gel column with absolute ethanol as the eluent, and the yield is 83%. ESI-MS: 459.4 (M+H).
[0046] 、Cis-[Ru(bpy) 2 (Cl) 2 ]·2H 2 O synthesis
[0047] With embodiment 1.
[0048] 、Cis-[Ru(phen) 2 (Cl) 2 ]·2H 2 O synthesis
[0049] With embodiment 1.
[0050] 、[Ru(bpy) 2 HAIP]·(PF 6 ) 2 preparation of
[0051...
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