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Double-core Gd complex and preparation method and applications thereof
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A technology of complexes and uses, applied in pharmaceutical formulations, organic chemistry methods, chemical instruments and methods, etc., can solve the problems of reduced signal-to-noise ratio, shortened imaging window time, and affected imaging quality applications, and achieves wide application prospects, excellent Effects of physicochemical properties
Active Publication Date: 2020-02-18
NINGBO UNIV
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However, such small-molecule complexes have short blood circulation time and short residence time in tissues, resulting in shortened imaging window time and reduced signal-to-noise ratio, which affects their imaging quality and clinical application.
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Embodiment 1
[0026] Weigh gadolinium acetate hexahydrate Gd(Ac) 3 ·6H 2 O (0.442g, 1.0mmol), 2,2':6', 2"-terpyridine (0.233g, 1.0mmol), 2,2'-biphenyldicarboxylic acid (0.240g, 1.0mmol) placed in a circle Add 4.0mL of distilled water, 10mL of ethanol and 2.0mL of DMF to the bottom flask, stir, heat and reflux for 30min, then transfer the mixture to a stainless steel reactor at 90°C for 48h, cool to room temperature naturally, and separate by filtration to obtain a colorless block shaped crystals.
Embodiment 2
[0028] Weigh Gd(Ac) 3 ·6H 2 O (0.442g, 1.0mmol), 2,2':6', 2"-terpyridine (0.233g, 1.0mmol), 2,2'-biphenyl dicarboxylic acid (0.240g, 1.0mmol) placed in a circle Add 4.0mL of distilled water, 10mL of ethanol and 2.0mL of DMF to the bottom flask, stir, heat and reflux for 30min, then transfer the mixture to a stainless steel reactor at 120°C for 24h, cool naturally to room temperature, and separate by filtration to obtain a colorless block shaped crystals.
Embodiment 3
[0030] Weigh Gd(Ac) 3 ·6H 2 O (0.442g, 1.0mmol), 2,2':6', 2"-terpyridine (0.233g, 1.0mmol), 2,2'-biphenyl dicarboxylic acid (0.240g, 1.0mmol) placed in a circle Add 4.0mL of distilled water, 10mL of ethanol and 2.0mL of DMF to the bottom flask, stir, heat and reflux for 30min, then transfer the mixture to a stainless steel reactor at 110°C for 36h, cool naturally to room temperature, and separate by filtration to obtain a colorless block shaped crystals.
[0031] The colorless blocky crystals prepared in the above examples were subjected to X-raysingle crystaldiffraction analysis, and it was determined that the asymmetric structural unit of the complex was composed of a Gd(III) ion, a 2,2':6', 2”-terpyridine, a 2,2’-biphenyl dicarboxylate (L 2- ), one acetate, and one coordinated water molecule ( figure 1 ), its structural formula is [Gd(L)(tpy)(Ac)(H 2 O)], the crystalsystem is monoclinic, the space group is C2 / c, and the unit cell parameters α=90°, β=112.013°, γ=...
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Abstract
The invention discloses a double-core Gd complex and a preparation method and applications thereof. The complex is prepared through self-assembly reactions among following raw materials: gadolinium acetate, 2,2':6',2''-terpyridine, and 2,2'-biphenyldicarboxylic acid; the complex has a definite spatial structure and an accurate molecular formula; and the synthesis steps are simple. The asymmetricunit of the complex is composed of one Gd (III) ion, one 2,2':6',2''-terpyridine, one 2,2'-biphenyl dicarboxylic radical, one acetic radical, and one coordinated water molecule. The crystalsystem isa mono-clinic system; the space group is C2 / c, and the geometrical configuration is that the gadoliniumion is 9-coordinated. The prepared cobalt complex is a paramagnetic single-molecular magnet, hasexcellent magnetic properties, and has a wide application prospect as an additive material of a NMR contrast agent.
Description
technical field [0001] The invention belongs to the field of coordination chemistry, and specifically relates to a binuclear Gd complex, a preparation method and application thereof. Background technique [0002] Complexes are a relatively large category of compounds, which are widely used in daily life, industrial production, life science or clinical medicine, and have developed particularly rapidly in recent years. They are not only associated with inorganic compounds and organometallic compounds, but also with Cluster chemistry, coordination catalysis and molecular biology are closely connected or overlapped in the current frontier of chemistry. The earliest research on complexes began in 1798, when the French chemist Tasael first prepared CoCl with divalentcobalt salt, ammoniumchloride and ammonia water. 3· 6NH 3 , the bonding and properties of coordination compounds could not be explained at that time. In 1893, the Swiss chemist Werner summed up the previous theori...
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