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Dicyclanil medicine crystal form II and preparing method thereof

A technology of desiginil and drugs, applied in the field of medicinal chemistry, can solve the problems of insufficient stability of crystal form A, long reaction time and high temperature

Inactive Publication Date: 2014-09-10
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the crystal form A is not stable enough, and it is easy to convert into other crystal forms
G and C crystal forms are respectively made of A crystal form in water at 80°C for 16 hours and 40°C for 24 hours. The reaction time of these two crystal forms is too long and the temperature is high, which is not conducive to industrial production.

Method used

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  • Dicyclanil medicine crystal form II and preparing method thereof
  • Dicyclanil medicine crystal form II and preparing method thereof
  • Dicyclanil medicine crystal form II and preparing method thereof

Examples

Experimental program
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Effect test

preparation example Construction

[0044] The preparation steps of the crystal form II of decinil drug according to the present invention are as follows:

[0045] (1) Dissolve dexinil in N,N-dimethylformamide solvent, heat and dissolve until it reaches a supersaturated state, stir for 30-60 minutes, and filter;

[0046] (2) Use a thin film to seal the mouth of the container containing the decinil solution, set volatilization holes in the thin film, let it stand for 5-7 days for volatilization, and colorless flaky crystals begin to precipitate in the container, and the crystals are obtained by separating them.

[0047] The present invention further provides a specific preparation method of crystal form II of decinil drug: dissolve 1.3-1.7 mmol of decinil in N,N-dimethylformamide solvent, heat and stir on a stirrer for 30 minutes ~60min, filter; seal the mouth of the beaker with a film of plastic wrap, poke a few small holes in the film with a needle, and let it stand for 5-7 days to evaporate, and colorless flak...

Embodiment 1

[0048] Example 1: Synthesis of crystalline form II using decinil and N,N-dimethylformamide:

[0049] Weighing:

[0050] Add 300 mg of crystalline form A dexinil, and weigh it accurately with an analytical balance.

[0051] Drug substance dissolution:

[0052] Use a pipette to accurately measure 20ml of N,N-dimethylformamide into a 50ml beaker, and stir for 30min.

[0053] Saturated solution cooling crystallization method:

[0054] At 153°C, when there is still a small amount that cannot be dissolved, take out the stirring bar, filter it into a clean 50ml transparent glass vial with analytical filter paper, seal the bottle mouth with plastic wrap, prick a few small holes with a needle, and let it stand for volatilization . After about 7 days, flaky colorless transparent crystals were precipitated in the bottle.

[0055] Toxic test on pests: the selected pests are adults of cotton boll weevil

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Abstract

The invention belongs to the field of pharmaceutical chemistry and particularly relates to a novel dicyclanil medicine crystal form II suitable for medicine development and a preparing method thereof. The dicyclanil medicine crystal form II and the preparing method thereof are characterized by a N,N-dimethylformamide solvate of a dicyclanil medicine. The crystal space groups of the dicyclanil medicine crystal form II are a monoclinic system. One dicyclanil molecule and one N,N-dimethylformamide molecule are bonded through hydrogen bonds so as to form an elementary structure unit of the dicyclanil medicine crystal form II. A preparation process of the dicyclanil medicine crystal form II adopts the N,N-dimethylformamide as a solvent, and adopts a saturated-solution cooling crystallization method, wherein a solution is saturated due to volatilization by heating so that crystals precipitate in the process of the solvent cooling and volatilization. The dicyclanil medicine crystal form II is capable of preventing larvae of various flies, mosquitoes and fleas from developing to pupae or imagines, and the like, and is obviously improved in solubility, stability and bioavailability.

Description

technical field [0001] The invention belongs to the field of medicinal chemistry, and specifically relates to a novel crystal form II of decinil suitable for drug analysis and a preparation method thereof. Background technique [0002] Dicyclanil (dicyclanil) is also known as propyrid, chemical name: 4,6-diamino-2-cyclopropylaminopyrimidine-5-carbonitrile, molecular formula: C 8 h 10 N 6 , Dexanil is a new type of insect growth regulator, emphasizing the control and regulation of pest populations, it can selectively and effectively control pests, and can maintain normal natural ecology without causing environmental pollution. As a new generation of veterinary drug, it has a strong market demand. Because the drug is not easily tolerated and has low residual value, it has high ecological and social benefits and meets the requirements and goals of today's green pesticides. The structural formula is as follows: [0003] [0004] At present, the patent WO9910333A1 disclose...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D239/50
CPCC07D239/50
Inventor 孙柏旺葛书旺王秋翠杨丽静
Owner SOUTHEAST UNIV
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