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Methylpyrazine derivative biological methyl alcohol compound

A methylpyrazine and methanol solvate technology, which is applied in the field of methylpyrazine derivative methanolate, can solve the problem of less crystal eutectic structure, low yield, and lack of crystallographic characterization parameters of acipimus. And other problems, to achieve the effect of good stability and high purity

Active Publication Date: 2019-03-08
LUNAN PHARMA GROUP CORPORATION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, there are many related reports about acipimox, but mainly about its preparation, preparation, physical and chemical properties and pharmacological properties. There are few reports about its crystal eutectic structure. Patents US2005239803A1, CN 103508963A, etc. have reported The preparation method of acipimox, the patent CN86103304-2 obtains the acipimox precipitate of crystal shape, which is acipimox hydrate, and the yield is low
In previous reports, there were few reports on the crystal form of acipimus, and the crystallographic characterization parameters of acipimus were not mentioned

Method used

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  • Methylpyrazine derivative biological methyl alcohol compound
  • Methylpyrazine derivative biological methyl alcohol compound
  • Methylpyrazine derivative biological methyl alcohol compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] Add 1g of methylpyrazine derivative sample to 5ml of methanol, heat to 50°C and stir to obtain a supersaturated solution, heat to reflux for 4 hours, stir and cool to crystallize (control the cooling rate at 0.3°C / min), and cool to 0 After ~5°C, keep the crystallization under temperature control for 48 hours, filter, rinse the filter cake with methanol, and dry in vacuum at 40°C for 3 hours to obtain methanol solvate crystals of methylpyrazine derivatives, with a yield of 96.33% and a purity of 99.96%. , Impurity I: 0.02%.

Embodiment 2

[0054] Suspend 1 g of methylpyrazine derivative powder sample in a mixed solvent (methanol 2.0ml + acetone 2.0ml), heat to 40°C and stir to obtain a supersaturated solution, heat to reflux for 3 hours, stir and cool to crystallize (control the cooling rate to 0.2 °C / min), after cooling down to -5~0 °C, stand for crystallization under temperature control for 36 hours, filter, wash the filter cake with methanol, and vacuum dry at 30 °C for 4 hours to obtain methylpyrazine derivative methanol solvate crystals , yield 95.56%, purity 99.94%, impurity I: 0.03%.

Embodiment 3

[0056] Suspend 1g of methylpyrazine derivative powder sample in a mixed solvent (methanol 1.0ml+purified water 4.0ml), heat to 60°C and stir to obtain a supersaturated solution, heat to reflux for 8 hours, stir and cool to crystallize (control the cooling rate to 0.5°C / min), after cooling down to 5-10°C, stand for crystallization under temperature control for 52 hours, filter, rinse the filter cake with ethanol, and vacuum-dry at 40°C for 5 hours to obtain methylpyrazine derivative methanol solvate crystals , yield 94.86%, purity 99.93%, impurity I: 0.04%.

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Abstract

The invention belongs to the technical field of medicine and specifically provides a methylpyrazine derivative biological methyl alcohol compound, a preparation method thereof and application thereofin preparing blood fat reducing medicine. The prepared methylpyrazine derivative biological methyl alcohol compound disclosed by the invention is radiated by Cu-K alpha, and an X ray diffraction spectrogram represented by 2 theta has the characteristic peaks at the 5.4 + / -0.2 degree, 5.8+ / -0.2 degree, 6.2+ / -0.2 degree, 7.7+ / -0.2 degree, 9.3+ / -0.2 degree and 27.7+ / -0.2 degree positions. The purityof the prepared methylpyrazine derivative biological methyl alcohol compound disclosed by the invention is higher than 99.9%; after the methylpyrazine derivative biological methyl alcohol compound ina solid state is tested under light, high temperature and high moisture, the purity is higher than 99.5%, and product stability is good. The methylpyrazine derivative biological methyl alcohol compound disclosed by the invention has the advantages of simple preparation technology and better industrial application prospect.

Description

technical field [0001] The invention belongs to the technical field of organic drug eutectics, in particular to a methanolate of a methylpyrazine derivative. Background technique [0002] Drug co-crystals are based on the principle of supramolecular chemistry, that is, molecular recognition and supramolecular self-assembly through intermolecular synergy. The active pharmaceutical ingredient (API) self-assembles with a suitable cocrystal former (CCF) through hydrogen bonds, or non-covalent bonds with saturation and directionality (such as van der Waals forces of aromatic hydrocarbons or benzene rings, π- π conjugation and halogen bond) to form a new structure, that is, drug co-crystal. It is based on hydrogen bonds, and neither needs to form new covalent bonds nor destroy existing covalent bonds. While retaining the pharmacological effects of the drug itself, it can also modify the physical and chemical properties of the drug, such as improving the Stability, reducing its h...

Claims

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Application Information

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IPC IPC(8): C07D241/24A61K31/4965A61P3/06C07C31/04C07C29/78
CPCA61P3/06C07D241/24C07B2200/13
Inventor 张贵民翟立海马庆文刘忠
Owner LUNAN PHARMA GROUP CORPORATION