CN102850278B - A kind of decoloring method of Anthelmintic imidazoles - Google Patents
A kind of decoloring method of Anthelmintic imidazoles Download PDFInfo
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- CN102850278B CN102850278B CN201210378848.9A CN201210378848A CN102850278B CN 102850278 B CN102850278 B CN 102850278B CN 201210378848 A CN201210378848 A CN 201210378848A CN 102850278 B CN102850278 B CN 102850278B
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Abstract
The invention discloses a kind of decoloring method of Anthelmintic imidazoles, comprise the following steps in order: Anthelmintic imidazoles is dissolved in acid by (1), be stirred to clearly molten; (2) in the above-mentioned clear liquid dissolved, add reductibility discoloring agent, be warming up to 40 ~ 55 DEG C, be incubated 1 ~ 2 hour; (3) in destainer, add solvent, fully stir, be cooled to crystallize out after room temperature, finally, centrifuge washing is dried and is obtained product.The invention has the advantages that: adopt reductibility discoloring agent to decolour to Anthelmintic imidazoles, overcome the drawback of traditional active carbon discoloring agent, decoloring method of the present invention is effective, easy to operate, is applicable to industrial application.
Description
Technical field
The present invention relates to a kind of decoloring method, be specifically related to the decolouring novel method of imidazoles parasiticide bulk drug.
Background technology
The synthetic intermediate of Anthelmintic imidazoles be all band O-Phenylene Diamine (
) material of this class intermediate structure, in reaction process, its easy oxidation by air is nitro or even the coloured material of azo band, cause final finished with pink or micro-yellow, instead of original off-white color or white, and the colored oxide compound generated in this building-up process, due in structure and polarity and finished product more approximate, be difficult to remove at the refining step of later separation leaching process according to routine, the appearance color of the finished product can be affected.
The appearance color of medicine is one of project of drug standard, reflects the purity of medicine to a certain extent.Now, require also more and more higher to the color appearance of medicine in the world, the former medicine particularly directly taking and inject class medicine requires also stricter.Therefore, the emphasis that medicine decoloring method also becomes research is investigated.At present, industrial conventional decolouring means mainly use charcoal absorption to decolour, and shortcoming is, this method can only be adsorbed the fine particle that is insoluble to solvent and to its species adsorbs DeGrain, can not solve pigment residue problem from basic.
Summary of the invention
The object of this invention is to provide a kind of decoloring method of Anthelmintic imidazoles of simple to operate, safety in production.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is: a kind of decoloring method of Anthelmintic imidazoles, comprises the following steps in order:
(1) Anthelmintic imidazoles is dissolved in acid, is stirred to clearly molten;
(2) in the above-mentioned clear liquid dissolved, add reductibility discoloring agent, be warming up to 40 ~ 55 DEG C, be incubated 1 ~ 2 hour;
(3) in destainer, add solvent, fully stir, be cooled to crystallize out after room temperature, finally, centrifuge washing is dried and is obtained product.
Further, in step (1), Anthelmintic imidazoles is selected from fenbendazole, Flubendazole, oxfendazole or the third foster imidazoles, and acid is selected from hydrochloric acid, sulfuric acid, formic acid, acetic acid, propionic acid, butyric acid, and the consumption of described acid is 1 ~ 10 times of Anthelmintic imidazoles weight ratio.
Further, in step (1), acid is acetic acid, take Anthelmintic imidazoles as radix, and the consumption of described acid is 2 ~ 3 times of Anthelmintic imidazoles weight ratio.
Further, suddenly in (2), reduction-decolor agent is selected from following reagent: any one of thiourea peroxide, sodium bisulfite, V-Brite B, oxalic acid, S-WAT, Sulfothiorine, ferrous ammonium sulphate, xitix, and the consumption of described discoloring agent is 0.1% ~ 20% of Anthelmintic imidazoles weight ratio.
Further, reductibility discoloring agent is preferably thiourea peroxide or V-Brite B, and the consumption of described discoloring agent is 2.0 ~ 5.0% of Anthelmintic imidazoles weight ratio.
Further, in step (3), solvent is selected from water or ethanol, methyl alcohol, Virahol, propyl carbinol, and described solvent load is 2 ~ 10 times of Anthelmintic imidazoles weight ratio.
Further, in step (3), solvent is water or ethanol, and described solvent load is 3 ~ 5 times of Anthelmintic imidazoles weight ratio.
The invention has the advantages that: adopt reductibility discoloring agent to decolour to Anthelmintic imidazoles, overcome the drawback of traditional active carbon discoloring agent, decoloring method of the present invention is effective, easy to operate, is applicable to industrial application.
Embodiment
Technical spirit of the present invention and beneficial effect can be fully understood in order to make the public; applicant will describe in detail the specific embodiment of the present invention below by reference to the accompanying drawings; but applicant is not the restriction to technical scheme to the description of embodiment, any changing in the form rather than substance according to the present invention's design all should be considered as protection scope of the present invention.
Embodiment 1
Step 1: in 500 milliliters of four-hole boiling flasks with thermometer and whipping appts, open and stir, adding 50g color is successively peach Anthelmintic imidazoles fenbendazole, adds the formic acid of 2 times of weight ratios, be stirred to clearly molten under normal temperature.
Step 2: the thiourea peroxide adding 2.0% weight ratio in complete molten clear solution, molten clear after be warming up to 40 ~ 50 DEG C, be incubated 1 hour.
Step 3: the ethanol adding 4 times amount in 40 ~ 50 DEG C of destainers, after fully stirring, is cooled to room temperature, product is slowly separated out, and centrifuge washing, dries to obtain finished product 46.3g, and color is off-white color, and yield is 92.6%.
Embodiment 2
Step 1: in 1000 milliliters of four-hole boiling flasks with thermometer and whipping appts, open and stir, adding 100g color is successively peach Anthelmintic imidazoles fenbendazole, adds the formic acid of 2.5 times of weight ratios, be stirred to clearly molten under normal temperature.
Step 2: the thiourea peroxide adding 3.0% weight ratio in complete molten clear solution, molten clear after be warming up to 50 ~ 55 DEG C, be incubated 1 hour.
Step 3: the ethanol adding 4.5 times amount in 50 ~ 55 DEG C of destainers, after fully stirring, is cooled to room temperature, product is slowly separated out, and centrifuge washing, dries to obtain finished product 94.3g, and color is off-white color, and yield is 94..3%.
Embodiment 3
Step 1: in 1000 milliliters of four-hole boiling flasks with thermometer and whipping appts, open and stir, adding 100g color is successively peach Anthelmintic imidazoles fenbendazole, adds the formic acid of 2.5 times of weight ratios, be stirred to clearly molten under normal temperature.
Step 2: the thiourea peroxide adding 3.5% weight ratio in complete molten clear solution, molten clear after be warming up to 40 ~ 45 DEG C, be incubated 1.5 hours.
Step 3: the ethanol adding 4 times amount in 50 ~ 55 DEG C of destainers, after fully stirring, is cooled to room temperature, product is slowly separated out, and centrifuge washing, dries to obtain finished product 93.8g, and color is off-white color, and yield is 93.8%.
Claims (6)
1. a decoloring method for Anthelmintic imidazoles, comprises the following steps in order:
(1) be dissolved in acid by Anthelmintic imidazoles, be stirred to clearly molten, described acid is selected from hydrochloric acid, sulfuric acid, formic acid, acetic acid, propionic acid, butyric acid;
(2) in the above-mentioned clear liquid dissolved, add reductibility discoloring agent, be warming up to 40 ~ 55 DEG C, be incubated 1 ~ 2 hour;
(3) in destainer, add solvent, fully stir, be cooled to crystallize out after room temperature, finally, centrifuge washing is dried and is obtained product, and described solvent is selected from water or ethanol, methyl alcohol, Virahol, propyl carbinol;
In step (2), reduction-decolor agent is selected from following reagent: any one of thiourea peroxide, sodium bisulfite, V-Brite B, oxalic acid, S-WAT, Sulfothiorine, ferrous ammonium sulphate, xitix, and the consumption of described discoloring agent is 0.1% ~ 20% of Anthelmintic imidazoles weight.
2. according to the decoloring method of the Anthelmintic imidazoles described in claim 1, it is characterized in that, in step (1), Anthelmintic imidazoles is selected from fenbendazole, Flubendazole, oxfendazole or Oxibendazole, and the consumption of described acid is 1 ~ 10 times of Anthelmintic imidazoles weight.
3. the decoloring method of Anthelmintic imidazoles according to claim 2, is characterized in that, in step (1), acid is acetic acid, take Anthelmintic imidazoles as radix, and the consumption of described acid is 2 ~ 3 times of Anthelmintic imidazoles weight.
4. according to the decoloring method of the Anthelmintic imidazoles described in claim 1, it is characterized in that, reductibility discoloring agent is preferably thiourea peroxide or V-Brite B, and the consumption of described discoloring agent is 2.0 ~ 5.0% of Anthelmintic imidazoles weight.
5. according to the decoloring method of the Anthelmintic imidazoles described in claim 1, it is characterized in that, in step (3), described solvent load is 2 ~ 10 times of Anthelmintic imidazoles weight.
6. the decoloring method of Anthelmintic imidazoles according to claim 5, is characterized in that: in step, and solvent is water or ethanol, and described solvent load is 3 ~ 5 times of Anthelmintic imidazoles weight.
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| CN104003867B (en) * | 2014-05-22 | 2015-08-05 | 江苏宝众宝达药业有限公司 | Method for recovering p-hydroxyphenylacetic acid from waste liquid |
| CN105601572B (en) * | 2016-01-22 | 2018-06-08 | 江苏宝众宝达药业有限公司 | A kind of preparation process of carbendazim |
| CN105732512A (en) * | 2016-04-11 | 2016-07-06 | 江苏泰仓农化有限公司 | Carbendazim production technology |
| CN109455712B (en) * | 2018-12-07 | 2022-04-01 | 江苏浦士达环保科技股份有限公司 | Preparation process of medicinal decolorizing active carbon |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1147507A (en) * | 1996-04-17 | 1997-04-16 | 常州市合成材料厂 | Prepn process of albendazole |
| CN1125055C (en) * | 2001-09-29 | 2003-10-22 | 昆山双鹤药业有限责任公司 | Sulfamethoxazole decoloring and refining process with sulfur dioxide and carbamide |
| CN102010377A (en) * | 2010-11-22 | 2011-04-13 | 天津市职业大学 | Method for preparing high-purity white 2-hydroxy quinoxaline crystal |
| CN101362770B (en) * | 2007-08-10 | 2011-08-31 | 上海新先锋药业有限公司 | Cefpirome sulfate preparation technology |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102241631A (en) * | 2010-05-13 | 2011-11-16 | 吉林省博大制药有限责任公司 | Method for preparing edaravone raw material |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1147507A (en) * | 1996-04-17 | 1997-04-16 | 常州市合成材料厂 | Prepn process of albendazole |
| CN1125055C (en) * | 2001-09-29 | 2003-10-22 | 昆山双鹤药业有限责任公司 | Sulfamethoxazole decoloring and refining process with sulfur dioxide and carbamide |
| CN101362770B (en) * | 2007-08-10 | 2011-08-31 | 上海新先锋药业有限公司 | Cefpirome sulfate preparation technology |
| CN102010377A (en) * | 2010-11-22 | 2011-04-13 | 天津市职业大学 | Method for preparing high-purity white 2-hydroxy quinoxaline crystal |
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Address after: 226500 No.10, Yuejiang Road, Changjiang Town, Rugao City, Nantong City, Jiangsu Province Patentee after: Jiangsu Baozhong Baoda Pharmaceutical Co.,Ltd. Address before: 226500 No.10, Yuejiang Road, Changjiang Town, Rugao City, Nantong City, Jiangsu Province Patentee before: JIANGSU BAOZONG & BAODA PHARMACHEM Co.,Ltd. |