Hemi-5-fluorocytosine salt, as well as preparation method and application thereof
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A technology of flucytosine salt and flucytosine, which is applied in the field of chemical pharmaceuticals to achieve the effects of high repeatability, simple preparation process and high crystal purity
Active Publication Date: 2014-08-06
SUZHOU INST OF NANO TECH & NANO BIONICS CHINESE ACEDEMY OF SCI
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In fact, no pharmaceutically acceptable hemi-5-fluorocytosine salt with good moisture stability has been reported so far
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[0028] In some embodiments of the present invention, the preparation method of the salt may include the following steps:
[0029] (1) At a certain temperature, 5-fluorocytosine and acesulfame potassium are completely dissolved in the solvent according to a certain molar ratio to form a supersaturated, saturated or nearly saturated state;
[0030] (2) Lower the temperature of the above mixed solution, let it stand or volatilize the solvent, and precipitate salt crystals;
[0031] (3) Vacuum drying the obtained crystals to obtain colorless transparent crystals or white powder is the final product.
[0032] Further, the aforementioned solvent may be selected from, but not limited to, one of water, methanol, ethanol, acetic acid or a mixed solvent in any proportion thereof.
[0033] In a preferred embodiment, the dissolution temperature of the raw materials such as 5-fluorocytosine and acesulfame potassium is room temperature to 80°C.
[0034] In a preferred embodiment, the init...
Embodiment 1
[0039] Example 1 Preparation of salt (semi-5-fluorocytosine salt, the same below): Weigh 0.2 mmol 5-fluorocytosine and 0.1 mmol acesulfame potassium, dissolve in 20 mL methanol at 40°C, and volatilize at 25°C after filtration to obtain Crystalline salt, yield 95%, XRD pattern as figure 2 shown.
[0040] Example 2 Salt preparation: Weigh 1 mmol 5-fluorocytosine and 0.5 mmol acesulfame K, dissolve in 15 mL water at room temperature, and volatilize at 60°C after filtration to obtain crystalline salt with a yield of 84%. Such as image 3 , as shown in 4.
Embodiment 3
[0041] Example 3 Single crystal preparation: Weigh 0.1 mmol 5-fluorocytosine and 0.1 mmol acesulfame potassium, dissolve in 15 mL methanol at 60°C, filter and volatilize at room temperature to obtain crystalline salt, and perform single crystal test at 153K, the structure is as follows Figure 5 shown.
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Abstract
The invention discloses hemi-5-fluorocytosine salt, as well as a preparation method and application thereof. The salt adopts acesulfame salt, and mainly composed of 5-fluorocytosine cation (FCH+), 5-fluorocytosine neutral molecule (FC) and acesulfame anion (AH-) according to the molar ratio of 1 to 1 to 1, the crystal cell of the salt belongs to an anorthic system, has the axial length a being equal to 7.2613(2)A, b being equal to 10.5289(3)A, and c being equal to 11.6662(4)A, and has the axial angle Alpha being equal to 66.8180(11) degrees, Beta being equal to 82.0220(12) degrees, and Gamma being equal to 78.5670(12) degrees. The hemi-5-fluorocytosine salt provided by the invention can effectively solve the problem of low moisture stability of the 5-fluorocytosine,and has excellent and effective medicine content and heat stability, the preparation technology of the hemi-5-fluorocytosine salt is simple, the operation is easy, the cost is low, poisonous solvent residue is avoided, meanwhile, the object molecule component serves as a sweetener, the medical mouthfeel can be improved, and the hemi-5-fluorocytosine salt is applicable to pharmaceutical industry.
Description
technical field [0001] The invention particularly relates to a 5-fluorocytosine salt and a preparation method thereof, belonging to the field of chemical pharmacy. Background technique [0002] More than 80% of pharmaceutical products are developed and applied in the form of solid oral dosage forms. The same drug substance can be developed into different solid state forms, such as: polymorphs, hydrates, solvates, salts and co-crystals. Different solid state forms have different physicochemical properties. Drug salt formation technology is widely used in the pharmaceutical industry to improve the physical and chemical properties of drugs. According to statistics, more than half of APIs are developed into their salt forms. [0003] The molecular formula for 5-fluorocytosine is C 4 h 4 FN 3 O, which is a widely used antibacterial drug, is mainly used in the treatment of infective endocarditis, urinary tract infection and lung infection. 5-fluorocytosine itself has no ant...
Claims
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Patent Type & Authority Applications(China)
IPC IPC(8): C07D239/47C07D291/06A61P31/10
CPCC07D239/47C07D291/06
Inventor 张海禄王林汪莲艳邓宗武
Owner SUZHOU INST OF NANO TECH & NANO BIONICS CHINESE ACEDEMY OF SCI
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