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Method for synthesizing disulfide bond containing organic matter and disulfide bond containing rare earth cluster compound coexisting crystalline material through one-pot method at normal temperature

A technology of disulfide bonds and clusters, which is applied in the field of preparation of crystalline materials, can solve significant problems and achieve the effects of simple method, novel and reasonable design, and simple and easy method

Inactive Publication Date: 2017-11-03
JIANGXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] However, the simultaneous synthesis of disulfide-bonded organic compounds and the synthesis of disulfide-bonded metal clusters has not been reported, and the reaction is carried out at room temperature, making this method of great significance

Method used

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  • Method for synthesizing disulfide bond containing organic matter and disulfide bond containing rare earth cluster compound coexisting crystalline material through one-pot method at normal temperature
  • Method for synthesizing disulfide bond containing organic matter and disulfide bond containing rare earth cluster compound coexisting crystalline material through one-pot method at normal temperature
  • Method for synthesizing disulfide bond containing organic matter and disulfide bond containing rare earth cluster compound coexisting crystalline material through one-pot method at normal temperature

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] (1) Put 93mg of 2-mercapto-3-pyridinecarboxylic acid in a beaker, add 20mL of water, and adjust the pH to 6 with 0.1M sodium hydroxide solution to obtain solution A;

[0034] (2) 127mg of terbium trifluoromethanesulfonate was mixed with 20mL of acetonitrile to obtain solution B;

[0035] (3) Solution A and solution B were mixed, and the resulting mixed solution was volatilized at room temperature to obtain light yellow transparent crystals of the new compound I, which is a crystalline material in which disulfide-bond-containing organic compounds and disulfide-bond-containing clusters coexist.

Embodiment 2

[0037] (1) Put 93 mg of 2-mercapto-3-pyridinecarboxylic acid in a beaker, add 10 mL of water, and adjust the pH to 6 with ammonia water to obtain solution C;

[0038] (2) 127mg of terbium trifluoromethanesulfonate was mixed with 20mL of acetonitrile to obtain solution D;

[0039] (3) Solution C and solution D were mixed, and the resulting mixed solution was volatilized at room temperature to obtain light yellow crystal rare earth coordination polymer II.

Embodiment 3

[0041] (1) Put 93mg of 2-mercapto-3-pyridinecarboxylic acid in a beaker, add 20mL of water, and adjust the pH to 6 with 0.1M sodium hydroxide solution to obtain solution A;

[0042] (2) Mix 107mg of terbium nitrate hexahydrate with 20mL of acetonitrile to obtain solution B;

[0043] (3) Solution A and solution B were mixed, and the resulting mixed solution was volatilized at room temperature to obtain light yellow transparent crystals of the new compound I, which is a crystalline material in which disulfide-bond-containing organic compounds and disulfide-bond-containing clusters coexist.

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Abstract

The invention relates to a disulfide bond containing organic matter and disulfide bond containing rare earth cluster compound coexisting crystalline material which is synthesized through a one-pot method by reacting 2-sulfydryl-3-picolinic acid and rare-earth salt and then volatilizing at normal temperature and a preparation method thereof. The method is characterized in that organic reaction and inorganic reaction are synchronously performed during the one-pot method, and an organic product and an inorganic product are obtained. The preparation method comprises the following steps: a) dissolving LnmXn (Ln is a trivalent rare earth ion) into a solvent for later use; b) adding a deprotonated 2-sulfydryl-3-picolinic acid solution to the solution obtained in step a); c) volatilizing the mixed solution at room temperature until a pale yellow crystal is separated out after a period of time; and d) filtering the obtained pale yellow crystal, and drying in the air. The method is simple and convenient to operate, reasonable in design, suitable for various rare earth ions and sulfydryl-containing ligands, free from expensive instruments and equipment, free from heating, and high in creativity and practicability.

Description

technical field [0001] The invention relates to the technical field of organic compounds containing disulfide bonds and rare earth clusters, in particular to a preparation method for synthesizing a crystalline material in which organic compounds containing disulfide bonds and clusters containing disulfide bonds coexist by using a normal temperature volatilization method. Background technique [0002] A disulfide bond is chemically a single covalent bond derived from the binding of a thiol. It is also called disulfide bond or disulfide bridge, and it is mainly used in the field of biochemistry at present. Its official name is persulfide, but it is rarely used. The disulfide bond is similar to peroxide (R-O-O-R), and its overall linkage is R-S-S-R. [0003] Disulfide bonds play an important role in the folding and stability of certain proteins, which are mostly secreted in the extracellular environment. Due to the reducing environment in most cell compartments, the disulfid...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/00C07D213/80
Inventor 曾承辉李浩然郑恺钟声亮李苑
Owner JIANGXI NORMAL UNIV
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