Method for preparing 2-nitryl-4-methylsulphonylbenzoic acid

A technology of methylsulfonylbenzoic acid and methylsulfonyltoluene is applied in the field of preparation of 2-nitro-4-methylsulfonylbenzoic acid, and can solve the problems of difficulty in losing electrons, low product yield, low HOMO energy and the like, To achieve the effect of easier reaction and less difficulty

Inactive Publication Date: 2018-10-30
枣阳天燕硅普材料有限公司
View PDF1 Cites 3 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, since there are two electron-withdrawing groups attached to the benzene ring of 2-nitro-4-thiamphenicol toluene, the HOMO energy of 2-nitro-4-thiamphenicol toluene is relatively low. It is difficult to lose el

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for preparing 2-nitryl-4-methylsulphonylbenzoic acid
  • Method for preparing 2-nitryl-4-methylsulphonylbenzoic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] S1: Mix 650kg of nitrate 2-nitro-4-thiamphenicol toluene with 2000kg of 70% sulfuric acid and 430kg of 65% nitric acid, stir evenly, and add 2kg of catalyst vanadium pentoxide to it, stir, and carry out oxidation reaction ; The tail gas nitric oxide generated during the reaction process is absorbed by water.

[0035] S2: Add 800kg of water to the mixed liquid prepared in S1, stir, and carry out hydrolysis reaction.

[0036] S3: Add 300kg of water to the mixture prepared in S2, stir, filter, and centrifuge to obtain about 600kg of crude product and 3447kg of mother liquor. The mother liquor is distilled to obtain water and sulfuric acid respectively, and the recovered water can be used for the hydrolysis reaction in S2, and can also be used to absorb the tail gas in S1; the recovered sulfuric acid can be used as the reactant sulfuric acid in S1.

[0037] S4: Add 220 kg of liquid caustic soda (40% sodium hydroxide) and 1500 kg of clear water to the crude product obtained...

Embodiment 2

[0043] S1: Mix 650kg of nitrate 2-nitro-4-thiamphenicol toluene with 1500kg of 70% sulfuric acid and 400kg of 65% nitric acid, stir evenly, and add 2kg of catalyst vanadium pentoxide to it, stir, and carry out oxidation reaction ; The tail gas nitric oxide generated during the reaction process is absorbed by water.

[0044] S2: Add 1000kg of water to the mixed liquid prepared in S1, stir, and carry out hydrolysis reaction.

[0045] S3: Add 300kg of water to the mixture prepared in S2, stir, filter, and centrifuge to obtain about 550kg of crude product and 3300kg of mother liquor. The mother liquor is distilled to obtain water and sulfuric acid respectively, and the recovered water can be used not only for the hydrolysis reaction in S2, but also for absorbing the tail gas in S1; the recovered sulfuric acid can be used as reactant sulfuric acid in S1.

[0046] S4: Add 220 kg of liquid caustic soda (45% sodium hydroxide) and 1500 kg of clear water to the crude product obtained i...

Embodiment 3

[0052] S1': Mix 650 kg of nitrate 2-nitro-4-thiamphenicol toluene with 10 kg of iron powder, mix and stir, and gradually add 300 kg of liquid bromine to it, stir and mix evenly, after the reaction, add 280 kg of sodium amide to it, The reaction was sufficient, and liquid products and iron powder precipitation remained in the container.

[0053] S1: Mix the liquid product in S1 with 2000kg of 70% sulfuric acid and 430kg of 65% nitric acid, stir evenly, and add 0.5kg catalyst vanadium pentoxide to it, stir, and carry out oxidation reaction; Nitrogen oxides are absorbed with water.

[0054] S2: Add 800kg of water to the mixed liquid prepared in S1, stir, and carry out hydrolysis reaction.

[0055] S3: Add 300kg of water to the mixture prepared in S2, stir, filter, and centrifuge to obtain about 850kg of crude product and 3300kg of mother liquor. The mother liquor is distilled to obtain water and sulfuric acid respectively, and the recovered water can be used for the hydrolysis re...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention relates to the technical field of organic synthesis, and particularly relates to a method for preparing 2-nitryl-4-methylsulphonylbenzoic acid, which can better improve the phenomena ofreaction difficulty and relatively low product yield caused by relatively high molecular oxidation potential in the process of oxidizing 2-nitryl-4-methylsulfonyl toluene. The method mainly comprisesthe following steps: mixing 2-nitryl-4-methylsulfonyl toluene with iron powder, adding liquid bromine into the mixture, and uniformly stirring and mixing; adding sodium amide into the mixture to sufficiently react, and using the final liquid product as a subsequent reacting material; mixing the liquid product with sulfuric acid and nitric acid, stirring, and performing an oxidation reaction undera catalyst condition; adding water into the mixed solution prepared in the above steps, and performing a hydrolysis reaction; adding water into the material prepared in the last step, filtering and centrifuging to respectively obtain a crude product and a stock solution; adding nitrous acid into the crude product, stirring and completely reacting; and adding sodium hypophosphite into the product in the last step, stirring, and completely reacting to obtain the product.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a preparation method of 2-nitro-4-thiamphenicol benzoic acid. Background technique [0002] 2-nitro-4-thiamphenicol benzoic acid is an important intermediate in organic synthesis, which is widely used in the production of dyes, medicines and pesticides. At present, the preparation of 2-nitro-4-thiamphenicol benzoic acid generally uses 2-nitro-4-thiamphenicol toluene as raw material, and the methyl on its benzene ring is oxidized to carboxyl, so as to prepare the corresponding acid. [0003] The Chinese invention patent with publication number CN106432006A discloses a nitration process of 2-nitro-4-thiamphenicol benzoic acid, which mainly prepares 2-nitro-4-thiamphenicol by mixing thiamphenicol toluene with nitric acid and sulfuric acid and stirring. 4-thiamphenicol benzoic acid. [0004] However, since there are two electron-withdrawing groups attached to the benzene...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
IPC IPC(8): C07C315/04C07C317/44
CPCC07C315/04C07C317/44C07C317/36C07C317/14
Inventor 李仁峰
Owner 枣阳天燕硅普材料有限公司
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap