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Preparation of nitrogen heterocyclic compound metal salt or its heterocyclic compound complex

A technology of nitrogen heterocyclic compounds and heterocyclic compounds, applied in lithium organic compounds, sodium organic compounds, organic chemistry, etc., can solve the problems of long time consumption, large solvent consumption, and difficulty in complete reaction balance

Active Publication Date: 2014-06-25
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the invention is to propose a practical method suitable for the preparation of various nitrogen heterocyclic compound metal salts, to overcome the large amount of solvent consumption in the prior art method, the complex operation process, long time-consuming and the existence of a balance in the reaction that is difficult to complete and other shortcomings

Method used

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  • Preparation of nitrogen heterocyclic compound metal salt or its heterocyclic compound complex
  • Preparation of nitrogen heterocyclic compound metal salt or its heterocyclic compound complex
  • Preparation of nitrogen heterocyclic compound metal salt or its heterocyclic compound complex

Examples

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Effect test

Embodiment 1

[0024] Embodiment 1: the preparation of imidazole sodium

[0025] In the glove box, weigh 687 mg of imidazole and 252 mg of sodium hydride in the same ball mill jar. Note that the two samples cannot be in contact at this time. After this ball mill jar is sealed, carefully transfer to the ball mill, under the condition of 50 ℃, under the rotating speed of 200rpm, ball mill for 5 hours. The degree of progress of the reaction can be realized by monitoring the pressure change in the ball mill tank. figure 1 It is the X-ray diffraction (XRD) spectrum of the prepared sample. It can be seen that it is consistent with the diffraction peak of imidazole sodium in the database, which proves that we have synthesized imidazole sodium and illustrates the feasibility of this preparation method.

Embodiment 2

[0026] Embodiment 2: the preparation of imidazole lithium

[0027] In the glove box, weigh 687 mg of imidazole and 81 mg of lithium hydride in the same ball mill jar. Note that the two samples cannot be in contact at this time. After this ball mill jar is sealed, carefully transfer to the ball mill, under the condition of 50 ℃, under the rotating speed of 200rpm, ball mill for 20 hours. The degree of progress of the reaction can be realized by monitoring the pressure change in the ball mill tank. figure 2 For the X-ray diffraction (XRD) spectrum of the prepared sample, it can be seen that the diffraction peaks of imidazole and lithium hydride have disappeared, replaced by a new set of diffraction peaks, which proves that a new species has been formed, namely our The target product is lithium imidazole.

Embodiment 3

[0028] Embodiment 3: the preparation of pyrrole sodium, pyrrole lithium

[0029] In the glove box, weigh 252 mg of sodium hydride (or 81 mg of lithium hydride), and measure 0.5 ml of pyrrole in the same ball mill jar. Note that the two samples cannot be in contact at this time. After the ball mill jar was sealed, it was carefully transferred to a ball mill, and ball milled at 150 rpm for 5 hours at room temperature. The degree of progress of the reaction can be realized by monitoring the pressure change in the ball mill tank. image 3 X-ray diffraction (XRD) spectra of the prepared pyrrole sodium and pyrrole lithium powder samples.

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Abstract

The invention relates to a synthetic method for preparing nitrogen heterocyclic compound metal salt and nitrogen heterocyclic compound metal salt heterocyclic compound complex. Under a solvent-free condition, nitrogen heterocyclic compounds are mixed with corresponding metal hydrides, and ball milling is carried out to obtain corresponding nitrogen heterocyclic compound metal salt; under the solvent-free condition, ball milling of a mixture of the nitrogen heterocyclic compounds, the corresponding metal hydrides, and heterocyclic compound ligands according to a certain ratio is carried out, or ball milling of a mixture of the nitrogen heterocyclic compound metal salt and a certain amount of heterocyclic compound ligands is carried out, so as to obtain nitrogen heterocyclic compound metal salt heterocyclic compound complex. The ball milling temperature is generally between -100 DEG C and 300 DEG C; the rotating speed is between 10 rpm and 500 rpm; the ball milling time is generally controlled to be 1-300 hours. The preparation method has the advantages of simplicity, practicality, no solvent, no reaction balance point, reaction thoroughness, reaction process monitorability, and easy amplification.

Description

technical field [0001] The invention belongs to the field of preparation method technology and the preparation of unknown compounds, and in particular relates to the preparation of nitrogen heterocyclic compound metal salts (such as: imidazole sodium) and heterocyclic compound complexes (such as: imidazole sodium·imidazole) based on ball milling. Background technique [0002] Nitrogen heterocyclic compounds refer to cyclic organic compounds containing nitrogen heteroatoms in the ring structure, and most of them are basic. Many biologically active compounds are nitrogen heterocyclic compounds, such as vitamin B1, histidine, nitrogenous bases of DNA (ATCG) and so on. So nitrogen heterocyclic compounds have always been the focus of attention in the fields of organic synthesis and medicine. [0003] Metal salts of nitrogen heterocyclic compounds are a class of intermediates that are often used in the process of synthesizing nitrogen heterocyclic compound derivatives, especially...

Claims

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Application Information

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IPC IPC(8): C07D233/58C07D207/323C07F1/04C07F1/02
CPCC07D207/323C07D233/58
Inventor 陈萍刘彬熊智涛吴国涛何腾
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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