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A kind of preparation method of 5-fluorouracil spherical crystal

A technology of fluorouracil and spherical crystals, which is applied in the field of preparation of 5-fluorouracil spherical crystals, can solve problems such as solvent or reagent residue, and achieve the effects of increasing shear force and breaking force, reducing aggregation efficiency, and large wetting angle

Active Publication Date: 2019-11-08
JINGHUA PHARMA GRP NANTONG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Most of these methods need to introduce other solvents or reagents such as good solvents, poor solvents or bridging agents, which easily lead to the residue of solvents or reagents.

Method used

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  • A kind of preparation method of 5-fluorouracil spherical crystal
  • A kind of preparation method of 5-fluorouracil spherical crystal
  • A kind of preparation method of 5-fluorouracil spherical crystal

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preparation example Construction

[0028] The preparation method of 5-fluorouracil spherical crystal of the present invention, this preparation method comprises the following steps:

[0029] (1) Add 5-fluorouracil and purified water solvent into a cylindrical reactor, and heat to 90-100°C under stirring to prepare a 5-fluorouracil solution;

[0030] (2) Decrease the temperature and crystallize the 5-fluorouracil solution in the step (1) at a stirring speed of 140-280rpm, and adopt a gradient cooling method to cool down for 4-5h;

[0031] (3) The temperature of the system is lowered to below 35° C. for filtration, and the filter cake is dried under normal pressure at 70-80° C. for 3-4 hours. After drying to constant weight, spherical crystals of 5-fluorouracil are obtained.

[0032] Among the present invention, the more specific implementation mode as an example is: the consumption of the purified water solvent in the step (1) is 10-15 times of 5-fluorouracil, and the stirring in the step (1) adopts a turbine ty...

Embodiment 1

[0035] Add 3kg of 5-fluorouracil and 30kg of purified water (10 times the mass of 5-fluorouracil) into a clean 50L cylindrical reactor, stir with a turbine-type stirring paddle, heat the reaction system to 100°C, and dissolve the solid completely to obtain 5 - Aqueous solution of fluorouracil.

[0036] The temperature of the above solution was lowered at a rate of 0.2°C / min under stirring at 240rpm. At 93°C, solids began to precipitate. As the temperature decreased, the amount of solids precipitated increased.

[0037] Filter when the temperature of the solution drops to 25°C, and wash the filter cake with purified water. Drying at 70° C. under normal pressure for 4 hours gave about 2.71 kg of 5-fluorouracil spherical crystal product with a yield of 90.33%.

[0038] The microscope appearance picture of the obtained product is as follows: figure 1 As shown, the obtained crystal is a regular ellipsoid shape; D(0.9)=965 μm of the product, and the particle size distribution diag...

Embodiment 2

[0040] Add 1.6kg of 5-fluorouracil and 24kg of purified water (15 times the mass of 5-fluorouracil) into a clean 30L cylindrical reaction kettle, stir with an impeller-type stirring paddle, heat the reaction system to 95°C, and dissolve the solid completely to obtain 5-fluorouracil aqueous solution.

[0041] The temperature of the above solution was lowered at a rate of 0.3°C / min under stirring at 140rpm, solids began to precipitate at 90°C, and the amount of solids precipitated increased as the temperature decreased.

[0042] Filter when the temperature of the solution drops to 10°C, and wash the filter cake with purified water. After drying at 70°C under normal pressure for 4 hours, about 1.43 kg of spherical crystal product of 5-fluorouracil was obtained, with a yield of 89.37%.

[0043] The microscope appearance picture of the obtained product is as follows: figure 2 As shown, the obtained crystal is a regular ellipsoid shape; the D(0.9)=921 μm of the product, and the p...

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Abstract

The invention relates to a method for preparing 5-fluorouracil spherical crystals. The method comprises the steps: adding 5-fluorouracil and purified water into a cylindrical reactor, and heating the temperature to 90 DEG C to 100 DEG C with stirring, so as to prepare a 5-fluorouracil solution; and subjecting the solution to cooling crystallization in a gradient cooling manner at a specific stirring rate, carrying out filtering when the temperature of a system is cooled to 35 DEG C or below, and drying a filter cake at the temperature of 70 DEG C to 80 DEG C until the weight of the filter cake is constant, thereby obtaining the 5-fluorouracil spherical crystals. The method has the advantages that the single purified water is adopted as a solvent, and the 5-fluorouracil spherical crystals are prepared under the condition of not adding other reagents, so that the problem of solvent residual is avoided; and the operation is simple, the filtering rate is high, and the fluidity of the product is good, so that industrial production is facilitated.

Description

technical field [0001] The invention belongs to the technical field of crystallization in the chemical engineering industry, and in particular relates to a method for preparing spherical 5-fluorouracil crystals. Background technique [0002] 5-Fluorouracil (CAS: 51-21-8), white crystal or powder, slightly soluble in water and slightly soluble in ethanol. Its English name is 5-Fluorouracil, its chemical name is 5-fluoro-2,4-dioxopyrimidine, and its molecular formula is C 4 h 3 FN 2 o 2 , the molecular weight is 130.08, and the structural formula is as formula (1). 5-Fluorouracil is a pyrimidine fluoride, which belongs to anti-metabolism and anti-tumor drugs. It can inhibit thymidine nucleotide synthetase, block the conversion of deoxypyrimidine nucleotides into thymidine nucleosides, and interfere with DNA synthesis. It also has a certain inhibitory effect on RNA synthesis. [0003] [0004] There are no relevant patents or reports on the preparation method of 5-fluo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D239/553
CPCC07D239/553
Inventor 朱春林滕飞沈小娟陈雪莲丛亚娟
Owner JINGHUA PHARMA GRP NANTONG
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