Production method of 1,2- benzisothiazole-3-ketone
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A technology of benzisothiazole and its production method, which is applied in the fields of air quality improvement and organic chemistry, can solve problems such as air pollution, increase in production cost, pollution, etc., and achieve the effects of avoiding pollution and reducing production cost
Inactive Publication Date: 2009-01-28
NANJING UNIV
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Problems solved by technology
At present, in the industrial route of using o-chlorobenzonitrile as raw material, sulfidation and chlorination of sodium methyl mercaptide to synthesize BIT, chlorobenzene is used as a solvent, and 1-1.4 tons of chlorobenzene is consumed per ton of product, which not only increases the production cost but also consumes Chlorobenzene enters the atmosphere and waste water causing air pollution and water pollution
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Embodiment 1
[0011] Add 100g of o-chlorobenzonitrile and 2g of catalyst tetrabutylammonium bromide into a four-neck flask, heat up to 50°C under stirring, then slowly add 200ml of 20% sodium methyl mercaptide solution dropwise to carry out vulcanization reaction, and drop it over in 4 hours , continue to react for 2h, cool and stand still, remove the lower aqueous phase, and wash the upper organic phase twice with 200ml of water;
[0012] Put the organic phase (102ml) obtained by the sulfidation reaction into an Erlenmeyer flask, add 30.6ml of water, feed 77.5g of chlorine gas under stirring, react for 2h, control the reaction temperature to 15°C with cooling water, and wait until the organic phase completely disappears After forming a powdery white suspended solid, filter and wash the filter cake twice with 200ml of water, and dry at 50°C for 5 hours to obtain 93.23g of BIT product with a purity of 98.6%, and a yield of 92%.
Embodiment 2
[0014] Add 50g of water, 100g of o-chlorobenzonitrile and 2g of catalyst tetrabutylammonium bromide into a four-necked flask, and under stirring, raise the temperature to 80°C and add 300ml of 20% sodium methyl mercaptide solution dropwise for vulcanization reaction, and drop it for 6 hours , continue to react for 6h, cool and stand still, remove the lower aqueous phase, and wash the upper organic phase twice with 200ml of water;
[0015] Put the organic phase (101ml) obtained by the sulfidation reaction into an Erlenmeyer flask, add 202ml of water, 103g of chlorine gas under stirring, react for 5h, control the reaction temperature to 30°C with cooling water, until the organic phase completely disappears to form a powdery white suspension After solid, filter and wash the filter cake twice with 200ml of water, dry at 80°C for 5h to obtain 94.75g of BIT product with a purity of 99.2%, and a yield of 93.5%.
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Abstract
A preparation method of 1, 2-benzisothiazole-3-ketone (BIT) is a BIT synthetic route realized by adopting a 2-chlorobenzonitrile method which selects water to replace chlorobenzene as a sulfurization and chlorination solvent. By adopting the method, the pollution of the chlorobenzene to atmosphere and water body is thoroughly eliminated and the total production cost of BIT is greatly reduced. The method comprises the following steps: chlorobenzonitrile is added with water accounting for 0-50% of the mass of the chlorobenzonitrile, and is added with a catalyst, then is added with sodium methyl mercaptide solution dropwise for a sulfuration reaction after heating, and the reactant is cooled for standing, a lower layer water phase is given out, water is added to rinse an upper layer organic phase, then the organic phase obtained in the sulfurization process is added with water accounting for 30%-200% of the volume of the organic phase; and chlorine is introduced into for reacting for 2-5h while stirring, then filtration is carried out to obtain a filter cake after the organic phase completely disappears and a white-pink suspended solid is produced, the filter cake is washed by clear water and is dried at low temperature to obtain the BIT product.
Description
technical field [0001] This method proposes a kind of production method of 1,2-benzisothiazol-3-ketone (BIT), specifically, a kind of o-chlorobenzonitrile method production that replaces chlorobenzene with water as the solvent of vulcanization and chlorination BIT method. Background technique [0002] 1,2-Benzisothiazol-3-one is mainly used as biological fungicide. At present, in the industrial route of using o-chlorobenzonitrile as raw material, sulfidation and chlorination of sodium methyl mercaptide to synthesize BIT, chlorobenzene needs to be used as a solvent, and the consumption of chlorobenzene per ton of product is 1-1.4 tons, which not only increases the production cost but also consumes Chlorobenzene enters the atmosphere and waste water causing air pollution and water pollution. Contents of the invention [0003] The present invention proposes a BIT synthesis route using water instead of chlorobenzene as a solvent for vulcanization and chlorination through the...
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