Ruthenium (II) porphyrin complex connected by flexible carbon chain and preparation method and application thereof
A technology of porphyrin complexes and complexes, applied in the field of ruthenium porphyrin complexes and their preparation, can solve the problems of strong toxicity and low activity
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Embodiment 1
[0041] Example 1Ru(bpy) 2 Synthesis of (4-p)POTPP
[0042] cis-[Ru(bpy) 2 Cl 2 ].H 2 Synthesis of O: RuCl 3 .nH 2 O, bipyridyl and lithium chloride in a three-necked flask, add 15ml of DMF, and reflux for 8h under the protection of argon. Cool to room temperature, add 50ml of acetone, freeze overnight. Suction filtration, the precipitate was washed several times with ice water and cold acetone, and dried in vacuum to obtain black microcrystals.
[0043] Synthesis of o-phenanthroline 5,6-dione: 1,10-phenanthroline, potassium bromide in a three-necked flask, slowly drop concentrated H under ice bath 2 SO 4 / concentrated HNO 3 Mix the acid in a three-necked flask. After the dropwise addition, react in an oil bath for 3 hours. After the reaction, ice water was added, the pH of the system was adjusted to close to 7 with NaOH, extracted with chloroform, and the chloroform was spin-dried to obtain yellow o-phenanthroline-5,6-dione.
[0044] Synthesis of 4-hydroxy-imidazo[...
Embodiment 2
[0050] Example 2Ru(phen) 2 Synthesis of (4-p)POTPP
[0051] cis-[Ru(phen) 2 Cl 2 ].H 2 Synthesis of O: See Example 1. Just replace the bipyridine in method 1 with o-phenanthroline to participate in the reaction.
[0052] 4-Hydroxy-imidazo[4,5-f][1,10]o-phenanthroline-diphenanthroline ruthenium Ru(phen) 2 Synthesis of p-Hpip: See Example 1.
[0053] Synthesis of 5-[4-(3-bromopentyloxy)phenyl]-10,15,20-triphenylporphyrin (p-POBrTPP): See Example 1.
[0054] 5-{4-{4'-Hydroxyimidazolium[1,10]o-phenanthroline-diphenanthroline ruthenium-pentyloxy}phenyl}-10,15,20-triphenylporphyrin [Ru( phen) 2 Synthesis of (4-p)POTPP]:
[0055] p-POBrTPP, Ru(phen) 2 p-Hpip was heated to reflux in DMF, and after cooling to room temperature, the solution was poured into saturated saline, left to stand for a while, suction filtered, washed with water several times, and vacuum-dried to obtain a purple crude product, which was purified by column chromatography and rinsed with chloroform. Coll...
Embodiment 3
[0057] Embodiment 3Ru(4,4'-Me)(bpy) 2 Synthesis of (4-p)POTPP
[0058] cis-[Ru(4,4'-Me)(bpy) 2 Cl 2 ].H 2 Synthesis of O: See Example 1. Just replace the bipyridine in method 1 with 4,4'-dimethylbipyridine to participate in the reaction.
[0059] 4-Hydroxy-imidazo[4,5-f][1,10]phenanthroline-(4,4'-dimethyl)bipyridine Ru(4,4'-Me)(bpy) 2 Synthesis of p-Hpip: See Example 1.
[0060] Synthesis of 5-[4-(3-bromopentyloxy)phenyl]-10,15,20-triphenylporphyrin (p-POBrTPP): See Example 1.
[0061]5-{4-{4'-Hydroxyimidazolium[1,10]phenanthroline-(4,4'-dimethyl)bipyridine ruthenopentyloxy}phenyl}-10,15,20 -Triphenylporphyrin [Ru(4,4'-Me)(bpy) 2 Synthesis of (4-p)POTPP]:
[0062] p-POBrTPP, Ru(4,4'-Me)(bpy) 2 p-Hpip was heated to reflux in DMF, and after cooling to room temperature, the solution was poured into saturated saline, left to stand for a while, suction filtered, washed with water several times, and vacuum-dried to obtain a purple crude product, which was purified by colum...
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