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Ruthenium polypyridyl complexes and synthesis method for derivatives thereof

A kind of synthetic method, the technique of ruthenium polypyridine, applied in the field of synthetic chemistry

Inactive Publication Date: 2008-07-09
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to provide a simple, high reaction rate synthetic method for ruthenium polypyridine complexes and derivatives thereof in order to solve the existing problems in the synthetic methods of ruthenium polypyridine complexes and derivatives thereof

Method used

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  • Ruthenium polypyridyl complexes and synthesis method for derivatives thereof
  • Ruthenium polypyridyl complexes and synthesis method for derivatives thereof

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Embodiment 1

[0047] Ru(dcbpy) 2 Cl 2 The synthesis, wherein dcbpy=2,2'-bipyridine-4,4'-dicarboxylic acid will 420mg of RuCl 3 ·3H 2 O and 791 mg of polypyridine ligand dcbpy (ie 2,2'-bipyridine-4,4'-dicarboxylic acid) were mixed in 150 ml of DMF (ie N,N-dimethylformamide), and loaded into a polytetrafluoroethylene In a stainless steel reactor lined with vinyl fluoride, high-purity N 2 Gas was bubbled for 15 minutes, dissolved oxygen was removed, the reactor was sealed, and heated to 190°C for 8 hours. After cooling, the resulting mixture was filtered, the filtrate was rotary evaporated to remove the DMF solvent, the obtained solid was recrystallized with acetone, the obtained crystal was filtered and vacuum-dried at 50°C for 3 hours to obtain the product Ru(dcbpy) 2 Cl 2 . Yield 85%.

[0048] Elemental analysis calculated value (C 24 h 16 N 4 o 8 Cl 2 Ru): C, 43.67; H, 2.44; N, 8.48; Cl, ​​10.74 (%). Measured values: C, 44.03; H, 2.50; N, 8.91; Cl, ​​10.70 (%).

Embodiment 2

[0050] Synthesis of cis-diisothiocyanato-bis(2,2'-bipyridyl-4,4'-dicarboxylic acid)ruthenium

[0051] Will Ru(dcbpy) 2 Cl 2 2H 2 O 850 mg was dissolved in 90 ml of DMF (protected from light), 60 ml of 0.1M NaOH aqueous solution was added thereto, 5.5 g of KSCN was dissolved in 10 ml of water and added to the above solution, and the resulting solution was loaded into a stainless steel tank with a Teflon lining In the reactor, with high-purity N 2 Gas was bubbled for 15 minutes to remove dissolved oxygen therein, the reactor was sealed, heated to 190° C., and kept for 6 hours under magnetic stirring conditions. After the reaction solution was cooled, the solvent was removed by rotary evaporation, and the resulting solid was dissolved in water and filtered through a sintered glass funnel, and the filtrate was washed with dilute HClO 4 Adjust the pH to 2.5, and after standing for 12 hours, suction filter to obtain a solid, and then use HClO with pH=3.5 4 Washed with aqueous s...

Embodiment 3

[0054] With embodiment 2 gained solid E, Ru(dcbpy) 2 (NCS) 2 Use LH-20 gel chromatographic column for chromatographic purification, using methanol as the eluent, the obtained dark purple band is recrystallized with ethanol to obtain Ru(dcbpy) 2 (NCS) 2 . Yield 70%.

[0055] Elemental analysis calculated value (C 26 h 16 N 6 S 2 o 8 Ru·2H 2 O): C, 42.1; H, 2.7; N, 11.3 (%). Measured values: C, 41.3; H, 2.7; N, 11.0 (%).

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Abstract

The invention belongs to the synthetic chemistry field, in particular to a synthesis process for ruthenium mixed-pyridine complex and derivative. Mixed-pyridine in ruthenium mixed-pyridine complex has two structures of (I) and (II), and the process comprises reacting ruthenium material and combined mixed-pyridine complex with various substituent position, complex kind (two teeth or three teeth, namely bipyridyl or terpyridyl material) and substituent property, and salt or water such as NCS, F, C1, Br, I and CN in a sealed reaction device which can be heated up and pressurized in one step or several steps for 0.5-48 hours under the temperature of 50-300 DEG C, thereby obtaining target product. The invention provides a high pressure synthesis process, which does not need a condensing reflux device, continuous inactive gas supply and inert atmosphere protection and has simple process. The process can increase reaction temperature over the boiling temperature of reaction solution in necessary, namely the boiling temperature relative to constant pressure, and has high reaction speed rate.

Description

technical field [0001] The invention belongs to the field of synthetic chemistry, in particular to a synthesis method of a ruthenium polypyridine complex and derivatives thereof. Background technique [0002] Ruthenium polypyridine complexes and their derivatives have the function of photolyzing water. These substances are used as light absorption sensitizers and light emission sensitizers, as well as in electrochemiluminescence, chemiluminescence, electron fluorescence transfer and nonlinear optics. Many fields have important roles. Such as N3 dyes used in dye-sensitized solar cells (ie [Ru(dcbpy) 2 (NCS) 2 ], wherein the ligand dcbpy=2,2'-bipyr-4,4'-dicarboxy), black dye (i.e. Ru(tctpy)(NCS) 3 , where tctpy=4,4',4"-tricarboxylic acid-2,2':6',2"-terpyridine) and so on. [0003] The existing synthesis methods of ruthenium polypyridine complexes and derivatives thereof generally use ruthenium chloride and other ruthenium source materials as starting materials, and carry o...

Claims

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Application Information

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IPC IPC(8): C07F15/00
Inventor 陈崧哲徐盛明徐刚李林艳
Owner TSINGHUA UNIV
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