Pyrazinamide derivatives as well as preparation method and uses thereof

A technology of bispyrazinamide and pyrazinecarboxylic acid, which is applied in the fields of organic compound synthesis and nano-device regeneration manufacturing

Inactive Publication Date: 2008-05-21
TIANJIN NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the prior art, the high ratio of organic compound molecules to water molecules forms crystals with a melting point of 60-61°C, and the research on the excellent reversible properties of adsorption and desorption of water molecules has not been reported in any literature. This characteristic of the compound is applied to the technology of recycling the silicon tip of the invalid atomic force microscope

Method used

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  • Pyrazinamide derivatives as well as preparation method and uses thereof
  • Pyrazinamide derivatives as well as preparation method and uses thereof
  • Pyrazinamide derivatives as well as preparation method and uses thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0059] (BPA) Synthesis of N,N'-(4-aza-1,7-heptyl)bispyrazinamide

[0060] Add 3.0 g (21.7 mmol) of methyl pyrazinecarboxylate into dry 20 mL of methanol under nitrogen protection, then add 10.0 mmol of dipropylenetriamine dropwise under nitrogen protection and vigorous stirring, and the reaction solution is heated to reflux under stirring for 10 h, spin Dry solvent, add methanol until the solute dissolves, add a small amount of activated carbon to decolorize, heat filter, pour into 20 times the amount of ice water, precipitate a white solid, vacuum filter under reduced pressure, wash the filter cake with a small amount of water, and use 100ml methanol: water to 10 :1 solution was recrystallized, allowed to stand at room temperature, crystals were precipitated naturally, filtered, and dried to obtain colorless crystals with a yield of 45%, melting point: 78.0-80.0°C.

Embodiment 2

[0062] The (BPA) synthesis of compound N, N'-(4-aza-1,7-heptyl)bispyrazinamide added 4.8g (35mmol) methyl pyrazinecarboxylate into dry 70mL methanol under nitrogen protection, Then under nitrogen protection and vigorous stirring, 17.0mmol dipropylenetriamine was added dropwise, the reaction solution was heated to reflux for 10h under stirring, the solvent was spin-dried, methanol solution was added until the solute was dissolved, a small amount of activated carbon was added for decolorization, hot filtration, poured into 20 times the amount A white solid was precipitated in ice water, filtered under reduced pressure, and the filter cake was washed with a small amount of water, recrystallized with a solution of 100ml methanol:water 10:1, left to stand at room temperature, and crystals were naturally precipitated, filtered, and dried to obtain Colorless crystals, yield 57%, melting point: 79.5-80.0°C.

[0063] Infrared analysis results:

[0064] The main infrared absorption pea...

Embodiment 3

[0071] Preparation of Hydrous Organic Compound Crystals

[0072] Dissolve 0.01mmol of N,N'-(4-aza-1,7-heptyl)bispyrazinamide in 10mL of methanol, add 0.01-1.0mL of water, magnetically stir to dissolve, mix well, and place it. Two weeks later, a colorless bulk crystal suitable for X-ray single crystal structure analysis was obtained (see accompanying drawing 4). Yield: 46%, melting point: 60-61°C.

[0073] Infrared analysis results:

[0074] The main infrared absorption peak is: IR(KBr, cm -1 ): 3255(m), 2868(m), 2740(m), 1649(s), 1515(s), 1477(m), 1424(m), 1317(m), 1161(s), 1058(s ), 865(m), 704(m), 657(s).

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Abstract

The present invention relates to a novel pyrazinamide derivative and more particularly a hydrated crystal of N, N'-(4-nitrogen heterocyclic-1, 7-heptyl) double-pyrazinamide compound, the structure and characteristic of which are mensurated by X-ray single-crystal diffraction, X-ray powder diffraction, thermogravimetric analysis, infrared spectrum, nuclear magnetism and element analysis; a molecular formula of the hydrated crystal is C8H18.50N3.50O5, the crystal belongs to the orthorhombic system, a space group is P2<1>2<1>2, unit cell parameters are that a is 11.164, b is 26.05, c is 4.582, and alpha, beta and gamma are equal to 90 degrees; unit cell size is that V is 1332.4 <3>. The preparation process of the hydrated crystal is simple; the crystal has high yield and purity and good stability. The pyrazinamide derivative can form a two-component crystal with the water absorption quantity of 29.56 percent, and the absorption of organic compound towards water molecule has the reversibility, which ensures that the compound can be applied to the recycling technology of worn atomic force microscopy silicon tips.

Description

technical field [0001] The invention belongs to the technical field of organic compound synthesis and nano device regenerative manufacturing technology, and relates to pyrazinamide derivatives and preparation methods thereof, especially N, N'-(4-aza-1,7-heptyl)bispyrazine Synthesis of amide and application of the compound in regeneration technology of silicon tip of invalid atomic force microscope. Background technique [0002] The chemical and physical quality characteristics of materials are mainly determined by their composition and the relative geometric positions of molecules, atoms, atomic groups or ions in a certain state, that is, the properties of substances depend on their composition and structure; the development of scientific theory and the progress of experimental technology and The perfection of detection methods provides the possibility to explore the microcosm. [0003] In the fields of science and technology such as electronics, biology, and energy develop...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D241/24G12B21/08G01N13/10G01Q70/16
Inventor 史学芳
Owner TIANJIN NORMAL UNIVERSITY
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