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Preparation method of 2-nitro-4-methyl sulfone benzoic acid

A technology of thiamphenicol benzoic acid and thiamphenicol toluene, which is applied in the field of one-pot synthesis of 2-nitro-4-thiamphenicol benzoic acid, which can solve incomplete reaction, large amount of three wastes, and difficult oxidation, etc. problems, to achieve the effect of improving oxidation capacity, simplifying production process and reducing acidic wastewater

Inactive Publication Date: 2015-01-07
JINZHOU KAICHUANG CHEM TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

This patented technology uses four different chemical reactions: 1) two steps are involved with producing 2-aminobenzonitrile (BEN), reducing manufacturing time and expenses;2) continuous use of sulphuric acid during the first step helps save on expensive materials while still providing effective results at lower temperatures than previous methods without this additionally requiring separate processes or equipment;3) utilizing copper salt instead of sulphone dichloroacetic acid as a promoter makes it easier to achieve higher yields compared to traditional methods due to its ability to reduce acidity by forming soluble salts that improve their effectiveness when mixed together with other reactants).4) making efficient and environment friendly degrading agents from H2O2.

Problems solved by technology

This patents describes methods for making certain substances from 2-aminothiachromanone (also called 1 - aminobenzimidazole) or another type of molecule known as tetrahydropathionatebenzoquinones. These compounds have various applications such as pharmaceutical products like antifungals, antihypercholesterolemics, immunosuppressants, etc., but they also find their importance due to their ability to function effectively within cells without causing harmful side effects during manufacturing processes.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 1. Preparation of oxidizing agent

[0028] Put 136g of concentrated sulfuric acid in a three-necked flask, and slowly add 68.0g (0.6mol) of 30% hydrogen peroxide solution dropwise therein under magnetic stirring. Heat will be released during the dropwise addition, and the temperature should be controlled below 30°C. , continue to stir for 20 min after the dropwise addition, and set aside.

[0029] 2, Preparation of 2-nitro-4-thiamphenicol benzoic acid

[0030] Add 17.02g (0.1mol) of 4-thiamphenicol toluene and 88.3g (0.883mol) of concentrated sulfuric acid into the three-necked flask, place the three-necked flask in a water bath, and slowly add 10.18g (0.105mol) of concentrated nitric acid dropwise to the three-necked flask. ), stirring constantly, and controlling the reaction temperature between 0 and 15°C, the dripping was completed in about 2.5 hours, and the reaction was continued for 0.6 hours after the addition was completed. If the nitration product is not sepa...

Embodiment 2

[0032] 1. Preparation of oxidizing agent

[0033] The concentrated sulfuric acid of 237.9g ​​is placed in the there-necked flask, and under magnetic stirring, slowly add 79.3g (0.7mol) concentration of 30% aqueous hydrogen peroxide solution therein, heat will be released during the dropping process, control the temperature at 30°C Next, continue to stir for 20 minutes after the dropwise addition is completed, and set aside.

[0034] 2, Preparation of 2-nitro-4-thiamphenicol benzoic acid

[0035] Add 17.02g (0.1mol) of 4-thiamphenicol toluene and 97.1g (0.971mol) of concentrated sulfuric acid into a three-necked flask, place the three-necked flask in a water bath, and slowly add 11.24g (0.116mol) of concentrated nitric acid dropwise to the three-necked flask ), stirring constantly, and controlling the reaction temperature between 0 and 15°C, the dripping was completed in about 2.5 hours, and the reaction was continued for 0.6 hours after the addition was completed. If the nit...

Embodiment 3

[0037] 1. Preparation of oxidizing agent

[0038] Place 68.0 g of concentrated sulfuric acid in a three-necked flask, and slowly add 68.0 g (0.6 mol) of 30% aqueous hydrogen peroxide dropwise therein under magnetic stirring. Heat will be released during the dropping process, and the temperature will be controlled at 30°C. Next, continue to stir for 20 minutes after the dropwise addition is completed, and set aside.

[0039] 2, Preparation of 2-nitro-4-thiamphenicol benzoic acid

[0040]Add 17.02g (0.1mol) of 4-thiamphenicol toluene and 79.5g (0.795mol) of concentrated sulfuric acid into the three-necked flask, place the three-necked flask in a water bath, and slowly add 9.21g (0.095mol) of concentrated nitric acid dropwise to the three-necked flask. ), stirring constantly, and controlling the reaction temperature between 0 and 15°C, the dripping was completed in about 2.5 hours, and the reaction was continued for 0.6 hours after the addition was completed. If the nitration p...

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PUM

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Abstract

The invention discloses a preparation method of 2-nitro-4-methyl sulfone benzoic acid. The preparation method comprises the following steps: preparing 2-nitro-4-methyl sulfone toluene in a concentrated sulfuric acid medium by using 4-methyl sulfone toluene as an initial material and nitric acid as a nitrating agent, directly adding water to dilute reaction liquid without separating the nitrating product of 2-nitro-4-methyl sulfone toluene, and dropping an oxidizing agent prepared by mixing hydrogen peroxide and concentrated sulfuric acid in the presence of a copper sulfate catalyst to prepare 2-nitro-4-methyl sulfone benzoic acid. The preparation method has the beneficial effects that 2-nitro-4-methyl sulfone benzoic acid is prepared by a one-pot process, so that the separation process of an intermediate is saved, the production process is simplified, the production cost is reduced, the yield is high, and the use amount of sulfuric acid and hydrogen peroxide is lowered. The preparation method is efficient, energy-saving, environment-friendly and more suitable for industrial production.

Description

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Claims

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Application Information

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Owner JINZHOU KAICHUANG CHEM TECH
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