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A nido-carborane containing organometallic compound crystal and a preparing method thereof

An organometallic and carborane technology, which is applied in the field of nested carborane-containing organometallic compound crystals and the preparation thereof, can solve the problems of high temperature, poor repeatability, low yield and the like, and achieves low cost and mild reaction conditions. , the preparation method is simple

Inactive Publication Date: 2017-04-19
SHANGRAO NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The object of the present invention is to provide a kind of nested carborane-containing organometallic compound crystal, which realizes that the boron atom is detached from the carborane parent under mild conditions to form a carborane derivative with a nested structure, which solves the problems existing in the prior art. The technical defects of high temperature, low yield, poor repeatability and strong polar solvents such as methanol or ethanol

Method used

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  • A nido-carborane containing organometallic compound crystal and a preparing method thereof
  • A nido-carborane containing organometallic compound crystal and a preparing method thereof
  • A nido-carborane containing organometallic compound crystal and a preparing method thereof

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Embodiment 1

[0023] Under the protection of argon, 1,2-dicarbo-closed-dodecaborane (86 mg, 0.6 mmol) was dissolved in 20 mL of anhydrous ether, and n-butyllithium (2.0 mol·L -1 Cyclohexane solution) (0.6mL, 1.2mmol), sulfur powder (38.4mg, 1.2mmol), after stirring and dissolving, add dichloro(p-methylisopropylphenyl) ruthenium (II) dimer (185mg, 0.3mmol) tetrahydrofuran solution 40mL, ice-water bath temperature control 0 ℃, after 4 hours of reaction, the solvent was dried under vacuum; after dissolving the product with 20mL chloroform, add HC≡CC(OH)(Ph) 2(124.8mg, 0.6mmol), after 20 hours of reaction at 30°C with temperature control, the reaction solution was concentrated to dryness; the target compound (179mg, 48%) was obtained by separation on a 200-300 mesh silica gel column (eluent: V (petroleum ether) ) / V (methylene chloride)=2:1); the compound was dissolved in a mixed solvent of n-hexane and methylene chloride for crystallization (V (hexane) / V (methylene chloride)=1:1), Obtain yello...

Embodiment 2

[0025] Under the protection of argon, 1,2-dicarbo-closed-dodecaborane (86 mg, 0.6 mmol) was dissolved in 20 mL of anhydrous ether, and n-butyllithium (2.0 mol·L -1 Cyclohexane solution) (0.6mL, 1.2mmol), sulfur powder (38.4mg, 1.2mmol), after stirring and dissolving, add dichloro(p-methylisopropylphenyl) ruthenium (II) dimer (185mg, 0.3mmol) tetrahydrofuran solution 40mL, ice-water bath temperature control 0 ℃, after 4 hours of reaction, the solvent was vacuum-dried; after dissolving the product with 20mL chloroform, add HC≡CC(OH)(Ph) 2 (124.8mg, 0.6mmol), after 18 hours of reaction at 35°C with temperature control, the reaction solution was concentrated to dryness; the target compound (183mg, 49%) was obtained by separation on a 200-300 mesh silica gel column (eluent: V (petroleum ether) ) / V (methylene chloride)=2:1); the compound was dissolved in a mixed solvent of n-hexane and methylene chloride for crystallization (V (hexane) / V (methylene chloride)=1:1), Obtain yellow blo...

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Abstract

The invention relates to a nido-carborane containing organometallic compound crystal and a preparing method thereof, and belongs to the technical field of organometallic chemistry. The structure of the compound is represented and determined by monocrystalline X-ray diffraction, nuclear magnetic resonance, and other methods. The crystal belongs to the monoclinic system and a space group P2<1> / n. The molecular formula of the crystal is C<27>H<37>B9ORuS2, and the molecular weight is 640.05. According to cell parameters, a is equal to 17.8494(15) angstroms, b is equal to 10.2272(9) angstroms, c is equal to 18.7853(16) angstroms, alpha is equal to 90 degrees, beta is equal to 92.9220 (10) degrees and gamma is equal to 90 degrees. 1,2-dicarba-closo-dodecaborane, n-butyllithium, sulfur powder, dichloro(p-cymene)ruthenium(II) dimer and 1,1-diphenyl-2-propyn-1-ol are adopted as raw materials and prepared under mild conditions into the nido-carborane containing organometallic compound that is (p-cymene)Ru(S2C2B9H<10>)(CH-C=C(Ph)<2>).H2O, wherein the p-cymene is 1-methyl-4-isopropyl phenyl. The compound has characteristics of the simple preparing method, a high yield, good repeatability, and the like and provides a novel idea for development of carborane-containing novel materials having good performance and application prospects.

Description

technical field [0001] The invention belongs to the technical field of organometallic chemistry, and in particular relates to a nested carborane-containing organometallic compound crystal and a preparation method thereof. Background technique [0002] Thanks to Li 2 E. 2 C 2 B 10 h 10 (E=S, Se) can act as a bidentate ligand to react with an organometallic reagent to form an organometallic compound containing a chalcogen-containing carborane. This type of compound not only has good chemical stability, solubility and crystallization properties, but also has aromaticity due to the five-membered metal heterocyclic ring with a nearly planar structure, and can be used as a model compound to study various organometallic chemical reactions. (eg: Meng X, Wang F S, Jin G X. Coord. Chem. Rev., 2010, 254, 1260; Hu J R, Wen J L, Wu D H, et al. Organometallics, 2011, 30, 298; Xie Z. Coord .Chem.Rev., 2006, 250, 259; Jin G X. Coord.Chem.Rev. 2004, 248, 587.) [0003] Studies have sh...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F15/00C07F5/02
CPCC07B2200/13C07F5/027C07F15/0046
Inventor 胡久荣黄蓉丽
Owner SHANGRAO NORMAL UNIV
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