Process method for synthesizing 1, 2-benzisothiazdin-3-ketone

A technology of benzisothiazoline and process method, applied in the direction of organic chemistry and the like, can solve the problems of a large amount of waste gas, high cost, long process route, etc., and achieve the effects of simplifying synthesis steps, reducing costs, and reducing environmental pollution

Inactive Publication Date: 2012-06-13
SHANGHAI YIMO BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The technical problem to be solved by the present invention is to provide a novel process for synthesizing 1,2-benzisothiaz...

Method used

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  • Process method for synthesizing 1, 2-benzisothiazdin-3-ketone
  • Process method for synthesizing 1, 2-benzisothiazdin-3-ketone
  • Process method for synthesizing 1, 2-benzisothiazdin-3-ketone

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Embodiment 1

[0036] Add 46.7 grams of o-chlorobenzonitrile, 30 grams of anhydrous sodium sulfide and 550 ml of DMF under nitrogen protection in a 1000 ml four-necked bottle, and react at 90 ° C for 3 hours. After the reaction is completed, cool down and distill the solvent DMF under reduced pressure. Add 500ml of water to the compound, filter with suction, place the filtrate in an ice-water bath, and acidify it to PH=2 with 10% hydrochloric acid, a yellow oily liquid appears in the lower layer, extract it with ethyl acetate, combine the organic matter, evaporate the solvent ethyl acetate, and obtain the product yellow liquid 32 gram.

[0037] Put 200 grams of o-mercaptobenzonitrile, 680 grams of chlorinated benzene, and 72 grams of water into a 1000 mL four-necked bottle, start stirring, cool down, control the temperature at 10°C-20°C, and pass chlorine gas, about 100 grams, and sample for liquid phase analysis When the peak of the raw material is 1%, continue to pass the chlorine until th...

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Abstract

The invention relates to a process method for synthesizing 1, 2-benzisothiazdin-3-ketone, which includes the steps: 1 enabling 2-chlorobenzonitrile and anhydrous sodium sulfide to react, and then performing acidification to obtain o-mercaptobenzonitrile; and 2 enabling the o-mercaptobenzonitrile to react with chlorine and water, cooling, crystallizing and obtaining target products. The process method adopts a 1, 2-benzisothiazdin-3-ketone synthesis method which is completely different from a traditional way, thereby greatly simplifying synthesis steps, lowering cost and reducing environment pollution simultaneously.

Description

[technical field] [0001] The invention belongs to the field of chemical synthesis, in particular to a process for synthesizing 1,2-benzisothiazolin-3-one. [Background technique] [0002] Biocides are used in a variety of applications to control or prevent the growth of microorganisms, thereby ensuring the preservation of products and materials. Industrial fungicides with 1,2-benzisothiazolin-3-one (CAS NR.2634-33-5, hereinafter referred to as BIT) as the main raw material have a very wide range of applications, such as in building materials industry, textile industry, It is widely used in leather industry, paper industry, electronics industry and food industry, as well as cosmetics and agriculture. [0003] Mainly use dithiosalicylic acid (DTSA) as raw material to prepare 1,2-benzisothiazolin-3-one at present, see figure 1 . In actual production, it can be seen from the following reaction formula that the acyl chloride of dithiosalicylic acid will produce a large amount o...

Claims

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Application Information

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IPC IPC(8): C07D275/04
Inventor 张静
Owner SHANGHAI YIMO BIOTECH
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