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Synthesis method for preparing saccharin

A synthesis method and saccharin technology, applied in organic chemistry and other directions, can solve the problems of many production links, long production process routes, and high ammonia nitrogen emissions, and achieve the effects of reducing emissions and treatment costs, reducing production costs, and avoiding process operations.

Active Publication Date: 2020-06-12
SHANGHAI JIAO TONG UNIV
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0003] It can be seen from the above that the existing technology not only has a long production process route, many production links, and high production costs, but also has a high ammonia nitrogen discharge in the production wastewater, and the organic wastewater and heavy metal ion wastewater are more difficult to treat.

Method used

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  • Synthesis method for preparing saccharin
  • Synthesis method for preparing saccharin
  • Synthesis method for preparing saccharin

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preparation example Construction

[0025] The synthetic method of preparing saccharin proposed by the present invention, its core is to carry out oxidation reaction of 1,2-benzisothiazolin-3-one compound and oxidizing agent, and oxidizing agent oxidizes 1,2-benzisothiazolin-3-one The thioether of compound is oxidized into sulfuramide, obtains o-benzoylsulfamide compound, and its reaction formula:

[0026]

[0027] Wherein, the R substituent is H or C 1 -C 8 Any substituent in straight-chain alkyl or branched-chain alkyl.

[0028] When specifically implementing the operation, the preferred embodiment can be carried out according to the following steps:

[0029] S1: Dissolve 1,2-benzisothiazolin-3-one compounds, salts, and alkalis in an organic solvent, stir, slowly add the oxidant dropwise, and stir after the dropwise addition is completed;

[0030] S2: Evaporate the solvent, add water, add acid dropwise, and adjust the pH value to 3-5;

[0031] S3: extracting the solution obtained in step S2, combining t...

Embodiment 1

[0034] Dissolve 15.1g (0.10mol) 1,2-benzisothiazolin-3-one, 0.206g (0.001mol) ruthenium trichloride, 4.0g (0.1mol) sodium hydroxide in 300mL ethanol, stir, drop slowly Add peracetic acid (20 mL). After 30 minutes of adding dropwise, stir for 6 hours. Evaporate the solvent, add 100mL of water, add hydrochloric acid dropwise, and adjust the pH value to 3. Extract 200mL×3 with ethyl acetate, combine the organic phases, dry over anhydrous sodium sulfate, filter with suction, and concentrate the filtrate to obtain brown-yellow o-benzoylsulfonimide (C 7 h 5 NO 3 Crude product of S), 19.7 g. The crude product was recrystallized with 150 mL of ethanol to obtain 10.6 g of light yellow solid, yield: 57.9%.

Embodiment 2

[0036] Dissolve 15.1g (0.10mol) of 1,2-benzisothiazolin-3-one, 0.230g (0.001mol) of silver oxide, and 4.0g (0.1mol) of potassium hydroxide in 300mL of acetonitrile, stir, and slowly drop over Hydrogen peroxide (20 mL). After 30 minutes of adding dropwise, stir for 6 hours. The solvent was evaporated, 100mL of water was added, and hydrochloric acid was added dropwise to adjust the pH value to 5. Extract 200mL×3 with ethyl acetate, combine the organic phases, dry over anhydrous sodium sulfate, filter with suction, and concentrate the filtrate to obtain brown-yellow o-benzoylsulfonimide (C 7 h 5 NO 3 The crude product of S) 19.2 g. The crude product was recrystallized with 150 mL of ethanol to obtain 9.6 g of light yellow solid, yield: 52.4%.

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Abstract

The invention provides a synthesis method for preparing saccharin, which comprises the following steps: carrying out an oxidation reaction on a 1,2-benzisothiazolin-3-one compound and an oxidant, andoxidizing thioether of the 1,2-benzisothiazolin-3-one compound into sulfamide by the oxidant, thereby obtaining the o-benzoyl sulfamide compound. Compared with a traditional saccharin production process, the saccharin synthesis method has the advantages of being simple in process, low in cost, efficient in separation, small in pollution and the like, and more conforms to green chemistry.

Description

technical field [0001] The invention relates to a new synthesis process of chemical products, in particular to a synthesis method for preparing saccharin. Background technique [0002] The traditional saccharin production process uses phthalic anhydride as raw material to prepare saccharin solution through eight steps of amidation reaction, esterification reaction, diazotization reaction, displacement reaction, chlorination reaction, ammoniation reaction, acid precipitation, and neutralization reaction. The solution is decolorized, concentrated, crystallized, dried and dried to obtain the finished saccharin product. The ammonification reaction in the traditional saccharin production process is to use ammonia water as a raw material, which reacts with methyl o-sulfonyl chloride benzoate obtained in the chlorination reaction to generate o-sulfonylbenzimide. Chinese patent CN201310703050.1, it uses phthalic anhydride as raw material through amidation reaction, esterification r...

Claims

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Application Information

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IPC IPC(8): C07D275/06
CPCC07D275/06
Inventor 张万斌申杰峰刘德龙
Owner SHANGHAI JIAO TONG UNIV
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