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Radical-metal complex type molecular ferromagnet and preparation method

A technology of metal complexes and free radicals, which is applied in the field of free radical-metal complex molecular ferromagnets and preparation, can solve the problems of difficult synthesis of three free radicals and low yield, and achieve easy composite processing and small size , the effect of light weight

Inactive Publication Date: 2004-11-10
NANKAI UNIV
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  • Abstract
  • Description
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AI Technical Summary

Problems solved by technology

This molecular ferromagnet is a complex of three free radicals and Mn(II), the synthesis of three free radicals is difficult and the yield is low

Method used

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  • Radical-metal complex type molecular ferromagnet and preparation method
  • Radical-metal complex type molecular ferromagnet and preparation method
  • Radical-metal complex type molecular ferromagnet and preparation method

Examples

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Embodiment 1

[0020] The synthesis of embodiment 1 free radical NITPhCl:

[0021] (1). Synthesis of 2,3-dimethyl-2,3-dinitrobutane (I) [L.W.Seigle, J.Org.Chem., 1940, 5, 100; P.Sayre, J.Am. Chem.Soc., 1955,71,6689] the NaOH solution of 45g (0.5mol) 2-nitropropane and 84ml 6N is added in the 500mL three-neck flask, ice-water bath cooling, mechanical stirring 0.5 hour, then slowly drip 40g ( 0.25mol) of liquid bromine, and then add 165ml of absolute ethanol, and continue to stir for 0.5 hours. It was then refluxed at 85°C for 3 hours, naturally cooled to room temperature, suction filtered, washed several times with distilled water, and dried to obtain 29 g of white flaky crystals with a yield of 65% and a melting point of 129-130°C.

[0022] Reaction formula:

[0023]

[0024] (2) Synthesis of 2,3-dimethyl-2,3-dihydroxyaminobutane (II) [M.Lamchem, J.Chem.Soc., 1966, 2300]

[0025] 10g NH 4 Dissolve Cl in 200ml of 1:1 ethanol-water solution, add 17.5g of product (I) under an ice-water b...

Embodiment 2

[0036] Example 2 manganese hexafluoroacetylacetonate Mn(hfac) 2 2H 2 Synthesis of O (P.A.Cotton J.Am.Chem.Soc., 1960, 82, 2979):

[0037] Weigh 4.8 grams of Mn(Ac) 2 2H 2 O, dissolved in 300ml 50% water-ethanol solution, added 200ml (10g) hfac, stirred, the solution turned yellow, evaporated, dried to obtain bright yellow flaky crystals. Yield: 68%.

Embodiment 3

[0038] Example 3 Synthesis and characterization of free radical-metal complexes:

[0039] (1) Synthesis: Add the Mn(hfac) synthesized above in the reaction vessel 2 2H 2 O 505mg, then add 100ml of anhydrous n-heptane, heat to boiling, cool down to 70°C after dissolving, add 50ml of anhydrous n-heptane solution containing 268mg NITPhCl free radical; after reacting for 10 minutes, cool down to room temperature, filter, and After standing for one week, green crystals were precipitated, and the yield was 51% (436 g).

[0040] (2). Determination of the structure of the complex

[0041] Select a green crystal with a size of about 0.10×0.20×0.25mm, use graphite monochromatized Mokα rays (λ=0.71073 ) as incident radiation on a BRUKER SMART 1000 X-ray diffractometer, and measure the temperature at 298 (2) K, the unit cell parameters were corrected by the least square method from 12911 diffraction points, and the crystal structure was solved by the SHELXL-97 direct method from the di...

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Abstract

The invention relates to a free radical - metallic complex type molecular ferromagnet and method for preparation wherein its chemical formula is [Mn(hfac)2(IMHPhC1)]#-[2] (NITPhC1), wherein hfac= hexafluoroacetylacetonato, IMHPhClú¢1- hydrogen-2-p- chlorphenyl-4, 4, 5, 5-tetramethyl-4, 5-dihydrogen-1-hydrogen-imidazole, and NITPhClú¢2--p- chlorphenyl-4, 4, 5, 5-tetramethyl imidazoline-3-oxidization-1-oxy free radical. According to the present invention, the process chooses single free radical synthesized molecular ferromagnet, which is a binuclear complex composed of the deacidized form of hexafluoroacetylacetonato manganese with free radicals, the binuclear complex and the NITPhCl free radical link an one-dimensional chain structure through the hydrogen bond.

Description

technical field [0001] The invention relates to a free radical-metal complex molecular ferromagnet and a preparation method. Background technique [0002] The research on free radical-metal complexes is at the intersection of chemistry, physics, materials and other disciplines. It is closely related to emerging disciplines such as coordination chemistry of free radicals, molecular electronics, magnetoelectronics, and molecular materials science. It is a very important topic in the world today. One of the active research fields [Jiang Zonghui et al., Chemical Bulletin, 5, 301, 2003] The so-called molecular ferromagnet refers to the compound that has the properties of a magnet at a certain temperature Tc synthesized by the method of preparing molecular compounds. The emergence of molecular ferromagnets has made it possible for magnetic materials composed of metal or ion lattices to be realized in solution chemistry under normal conditions in the form of molecular assemblies. ...

Claims

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Application Information

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IPC IPC(8): C07F15/00
Inventor 姜宗慧赵琦华阎世平
Owner NANKAI UNIV
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