CN103204823B - Method for purifying 1, 2-benzisothiazole-3-ketone - Google Patents
Method for purifying 1, 2-benzisothiazole-3-ketone Download PDFInfo
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- CN103204823B CN103204823B CN201310084775.7A CN201310084775A CN103204823B CN 103204823 B CN103204823 B CN 103204823B CN 201310084775 A CN201310084775 A CN 201310084775A CN 103204823 B CN103204823 B CN 103204823B
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Abstract
The invention belongs to the field of fine chemicals, and relates to a method for purifying 1, 2-benzisothiazole-3-ketone (BIT). Water-soluble polar proton solvents and water are mixed to form solvents to be re-crystallized so as to obtain snow-white granular 1, 2-benzisothiazole-3-ketone. The method particularly includes steps of mixing the water-soluble polar proton solvents with the water to obtain the solvents; mixing the obtained solvents with the 1, 2-benzisothiazole-3-ketone; heating a mixture of the solvents and the 1, 2-benzisothiazole-3-ketone until the mixture is dissolved completely; decoloring and filtering the mixture to obtain filter liquor; cooling the obtained filter liquor; filtering the filter liquor to obtain 1, 2-benzisothiazole-3-ketone crystals; and drying the obtained crystals. The method has the advantages that consumption of acid, alkali and a large quantity of water is omitted, pollution is greatly reduced, and the obtained products are high in quality and content, contain few impurities and are granular; as BIT has a severe irritation effect on respiratory ducts of human bodies and a BIT powder layer can be prevented from being inhaled by the human bodies, operation conditions are greatly improved; and the granular products are easy to dry, and production processes needing anhydrous BIT can be greatly facilitated as the granular products do not contain crystallization water.
Description
[technical field]
The invention belongs to field of fine chemical, relate to the method for purification of compound, specifically a kind of method of purification of 1,2-benzisothiazole-3-ketone.
[background technology]
1,2-benzisothiazole-3-ketone (BIT, formula I) is widely used in sterilant, sanitas, its traditional method of purification adopts acid-base method, with large water gaging for solvent, first dissolves with liquid caustic soda, then separate out with hydrochloric acid, obtain 1.2-benzisothiazole-3-ketone powder.But this method of purification has the following disadvantages: not only can produce a large amount of brine wastes, quality product is low, and dust is many, and operational condition is poor.
Therefore, if one can be provided to avoid using soda acid and large water gaging, decreasing pollution, and good product quality, content is high, greatly improves 1,2-benzisothiazole-3-ketone method of purification of operational condition, will have very important significance.
[summary of the invention]
Object of the present invention is exactly the method for purification that will solve above-mentioned deficiency and provide a kind of 1,2-benzisothiazole-3-ketone, not only avoid and uses soda acid and large water gaging, greatly reduce pollution, and products obtained therefrom quality is good, content is high, impurity is few, greatly improves condition.
The method of purification of a kind of 1,2-benzisothiazole-3-ketone of design for achieving the above object, comprises the following steps:
1) watersoluble polar protonic solvent is mixed with water make solvent, gained solvent and 1,2-benzisothiazole-3-ketone are mixed, is warming up to entirely molten, decolorization filtering, filtrate, described watersoluble polar protonic solvent is the combination of a kind of in methyl alcohol, ethanol or two kinds, wherein, 1,2-benzisothiazole-3-ketone and watersoluble polar protonic solvent mass ratio are 1.5-4.5, and water and 1,2-benzisothiazole-3-ketone mass ratio are 0-2; Obviously this watersoluble polar protonic solvent also can be one or more the combination in acetic acid, acetone, propyl alcohol, butanols, acetonitrile, formic acid;
2) gained filtrate is cooled, filter to obtain 1,2-benzisothiazole-3-ketone crystal, and dry gained crystal.
In certain preferred embodiments of the present invention, step 1) in 1,2-benzisothiazole-3-ketone and dissolution with solvents temperature be 40-120 DEG C.
In certain preferred embodiments of the present invention, step 2) in cooling temperature be 0-35 DEG C.
In certain preferred embodiments of the present invention, step 2) in the time of cooling be 1.5-8h.
In some embodiments of the present invention, step 2) in when cooling, stir filtrate, stirring velocity is 25-55RPM.
The present invention compared with the existing technology, there is following beneficial effect: to mix with water owing to adopting watersoluble polar protonic solvent and make solvent recrystallization, obtain snow-white particulate state 1,2-benzisothiazole-3-ketone, avoid and use soda acid and large water gaging, greatly reduce pollution; And on the one hand, products obtained therefrom quality is good, and content is high, and impurity is few, can meet some special purposes; On the other hand, products obtained therefrom is particulate state, can prevent BIT bisque from being sucked by human body, because the respiratory tract of BIT to people has serious hormesis, thus significantly improves operational condition; In addition, granular product is easily dry, after not being with crystal water, will have very large benefit to needing the production technique of the BIT of anhydrous state.
[accompanying drawing explanation]
Fig. 1 is that the HPLC of 1,2-benzisothiazole-3-ketone standard substance detects data;
Fig. 2 is that the HPLC of embodiment 1 products therefrom detects data.
[embodiment]
Below in conjunction with embodiment, following further illustrating is done to the present invention:
Experimental example 1
Throw 1,2-benzisothiazole-3-ketone 160g, methyl alcohol 450g, water 130g, be warming up to 65 DEG C complete molten, add 1.5g gac, insulation 30min, filters, gained filtrate, slow down stirring, slow cooling to 20 DEG C, about need 1h, filter, 100g cold water washing, dries to obtain the snow-white particle 1 of 145g, 2-benzisothiazole-3-ketone (HPLC>99.85%), yield 90.6%.
Experimental example 2
Throw 90% solid content 1,2-benzisothiazole-3-ketone 178g, methyl alcohol 450g, water 110g, be warming up to 66 DEG C complete molten, add 1.5g gac, insulation 30min, filters, gained filtrate, slow down stirring, slow cooling to 20 DEG C, about need 1h, filter, 100g cold water washing, dries to obtain the snow-white particle 1 of 143g, 2-benzisothiazole-3-ketone (HPLC>99.85%), yield 89.3%.
Experimental example 3
Throw 1,2-benzisothiazole-3-ketone 160g, ethanol 420g, water 135g, be warming up to 70 DEG C complete molten, add 1.5g gac, insulation 30min, filters, gained filtrate, slow down stirring, slow cooling to 20 DEG C, about need 1h, filter, 100g cold water washing, dries to obtain the snow-white particle 1 of 140g, 2-benzisothiazole-3-ketone (HPLC>99.85%), yield 87.5%.
Should be understood that; the present invention is not by the restriction of above-mentioned embodiment; change, the modification done under other any does not deviate from spirit of the present invention and principle, substitute, combine, simplify, all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (5)
1. a method of purification for 2-benzisothiazole-3-ketone, is characterized in that, comprises the following steps:
1) watersoluble polar protonic solvent is mixed with water make solvent, gained solvent and 1,2-benzisothiazole-3-ketone are mixed, is warming up to entirely molten, decolorization filtering, filtrate, described watersoluble polar protonic solvent is the combination of a kind of in methyl alcohol, ethanol or two kinds, wherein, 1,2-benzisothiazole-3-ketone and watersoluble polar protonic solvent mass ratio are 1.5-4.5, and water and 1,2-benzisothiazole-3-ketone mass ratio are 0.5-1.5;
2) gained filtrate is cooled, filter to obtain 1,2-benzisothiazole-3-ketone crystal, and dry gained crystal.
2. the method for claim 1, is characterized in that: step 1) in 1,2-benzisothiazole-3-ketone and dissolution with solvents temperature be 40-120 DEG C.
3. method as claimed in claim 1 or 2, is characterized in that: step 2) in cooling temperature be 0-35 DEG C.
4. method as claimed in claim 3, is characterized in that: step 2) in the time of cooling be 1.5-8h.
5. method as claimed in claim 4, is characterized in that: step 2) in when cooling, stir filtrate, stirring velocity is 25-55RPM.
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CN105753805A (en) * | 2016-03-31 | 2016-07-13 | 寿光新泰精细化工有限公司 | Method for purifying 1,2-benzisothiazole-3-ketone |
CN105801516B (en) * | 2016-04-28 | 2018-05-04 | 大丰跃龙化学有限公司 | A kind of 1,2- benzisothiazole-3-ketones purifying technique |
CN108794424A (en) * | 2018-07-16 | 2018-11-13 | 连云港市三联化工有限公司 | A kind of method for refining solvent of BIT |
CN109970677A (en) * | 2019-04-23 | 2019-07-05 | 中国烟草总公司郑州烟草研究院 | A kind of method of purification of 1,2-benzisothiazolin-3-one |
CN111559986A (en) * | 2020-06-22 | 2020-08-21 | 大连百傲化学股份有限公司 | Purification method of 1, 2-benzisothiazolin-3-ketone |
CN114181124B (en) * | 2021-12-13 | 2024-01-26 | 大连百傲化学股份有限公司 | Recycling treatment method of 1, 2-benzisothiazolin-3-one chlorination process wastewater |
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US4590196A (en) * | 1984-08-23 | 1986-05-20 | Bristol-Myers Company | Analgesic 1,2-benzisothiazol-3-ylpiperazine derivatives |
CA2151074C (en) * | 1994-07-05 | 2005-08-02 | Hirokazu Kagano | Method for producing 1,2-benzisothiazol-3-ones |
JP3777800B2 (en) * | 1998-06-24 | 2006-05-24 | 新日本理化株式会社 | Process for producing 1,2-benzisothiazol-3-ones |
US7585980B2 (en) * | 2006-05-25 | 2009-09-08 | Troy Corporation | Immobilized 1,2-benzisothiazolin-3-one |
JP2012214405A (en) * | 2011-03-31 | 2012-11-08 | Sumitomo Seika Chem Co Ltd | N,n'-methylenebis(1,2-benzisothiazolin-3-one) compound and method for producing the same |
CN102491955A (en) * | 2011-12-08 | 2012-06-13 | 上海易摩生物科技有限公司 | Process method for synthesizing 1, 2-benzisothiazdin-3-ketone |
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