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Four types of sulfuric acid nepresol organic drug eutectics and preparation method thereof

A kind of technology of bishydralazine and organic medicine, applied in the field of bishydralazine sulfate organic medicine co-crystal and preparation thereof

Inactive Publication Date: 2014-04-23
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Drug crystal form research and solid-state characterization of drugs are relatively mature and highly valued fields in the European and American pharmaceutical industry, but they are still in their infancy in the domestic pharmaceutical industry

Method used

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  • Four types of sulfuric acid nepresol organic drug eutectics and preparation method thereof
  • Four types of sulfuric acid nepresol organic drug eutectics and preparation method thereof
  • Four types of sulfuric acid nepresol organic drug eutectics and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] Synthesis of organic drug cocrystals using dihydralazine sulfate and 2,3-dihydroxybenzoic acid 1:

[0055] Raw material handling:

[0056] Accurately weigh 0.2mmol of hydralazine sulfate with an analytical balance, add 3ml of 2mol / L NaOH solution, stir for 30 minutes, then put the cloudy solution into a 5ml centrifuge tube, and centrifuge at a speed of 12000r / min for 3 minutes. The supernatant was removed, washed with water three times repeatedly, and put into a vacuum drying oven for drying.

[0057] Weighing:

[0058] The reactants are fed according to the ratio of dihydralazine: 2,3-dihydroxybenzoic acid = 1:2, and 0.2mmol dihydralazine and 0.4mmol 2,3-dihydroxybenzoic acid are accurately weighed with an analytical balance. Formic acid, all placed in clear glass vials.

[0059] Dissolution of API:

[0060] Accurately pipette 2ml of ethanol and 2ml of tetrahydrofuran into the glass vial with a 5ml pipette gun, stir for 30 minutes, the solution is in the state of w...

Embodiment 2

[0064] Synthesis of Organic Drug Cocrystal 2 Using Dihydralazine Sulfate and 2,4-Dihydroxybenzoic Acid:

[0065] Raw material handling:

[0066] Accurately weigh 0.2mmol of hydralazine sulfate with an analytical balance, add 3ml of 2mol / L NaOH solution, stir for 30 minutes, then put the cloudy solution into a 5ml centrifuge tube, and centrifuge at a speed of 12000r / min for 3 minutes. The supernatant was removed, washed with water three times repeatedly, and put into a vacuum drying oven for drying.

[0067] Weighing:

[0068] The reactants are fed according to the ratio of dihydralazine: 2,4-dihydroxybenzoic acid = 1:2, and 0.2mmol dihydralazine and 0.4mmol 2,4-dihydroxybenzoic acid are accurately weighed with an analytical balance. Formic acid, all in clear glass vials.

[0069] Dissolution of API:

[0070] Accurately pipette 1ml of ethanol and 3ml of tetrahydrofuran into the glass vial with a 5ml pipette gun, and stir for 30 minutes. The solution is in the state of white...

Embodiment 3

[0074] Synthesis of Organic Drug Cocrystal 3 Using Dihydralazine Sulfate and 2,5-Dihydroxybenzoic Acid:

[0075] Raw material handling:

[0076] Accurately weigh 0.2mmol of hydralazine sulfate with an analytical balance, add 3ml of 2mol / L NaOH solution, stir for 30 minutes, then put the cloudy solution into a 5ml centrifuge tube, and centrifuge at a speed of 12000r / min for 3 minutes. The supernatant was removed, washed with water three times repeatedly, and put into a vacuum drying oven for drying.

[0077] Weighing:

[0078] The reactants are fed according to the ratio of dihydralazine: 2,5-dihydroxybenzoic acid = 1:2, and 0.2mmol dihydralazine and 0.4mmol 2,5-dihydroxybenzoic acid are accurately weighed with an analytical balance. Formic acid, all in clear glass vials.

[0079] Dissolution of API:

[0080] Accurately pipette 2ml of ethanol and 2ml of tetrahydrofuran into the glass vial with a 5ml pipette gun, stir for 30 minutes, the solution is in the state of white tur...

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Abstract

The invention belongs to the technical field of organic drug eutectics, in particular to four types of sulfuric acid nepresol organic drug eutectics and a preparation method thereof. According to the invention, the method comprises the following steps that API (Active Pharmaceutical Ingredient) sulfuric acid nepresol is adopted to serve as the API, 2,3-dihydroxy-benzoic acid, 2,4-dihydroxy-benzoic acid, 2,5-dihydroxy-benzoic acid, and 2,6-dihydroxy-benzoic acid are adopted to serve as precursors, the ethanol and tetrahydrofuran serve as solvent, and a solvent evaporation method is adopted. According to the invention, as the organic solvent which has a low boiling point, is adopted, crystals can be separated out during the solvent evaporation, so as to obtain the four organic drug eutectics with novel structures. The organic drug eutectics prepared by the invention not only cures cardiovascular disease by a traditional API, but also has dramatic improvement in solubility, stability and bioavailability.

Description

technical field [0001] The invention belongs to the technical field of organic drug co-crystals, and in particular relates to four kinds of dihydralazine sulfate organic drug co-crystals and a preparation method thereof. Background technique [0002] In 1894, E. Fischer of Germany proposed the "lock-key" model based on the idea of ​​"selective interaction between molecules", which was the prototype of modern supramolecular science theory. In 1937, German K.L.Wolf et al. created the term "supramolecular" to describe highly ordered entities formed by the association of molecules. In a general sense, any collection of molecules has interactions, so people often refer to them as The structural level of matter aggregation state is called "supramolecular". It was not until 1978 that Professor J.M.Lehn of France finally proposed the complete concept of "supramolecular chemistry" based on the traditional research on the host-guest system rooted in organic chemistry. Supramolecular...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D237/34C07C65/05C07C51/41
Inventor 赵念张婷罗亚楠韩冰苏红敏贾江涛朱广山
Owner JILIN UNIV