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Method for preparing 2-nitro-4-methyl p-tolyl sulfone using solid superstrong acid

A technology of thiamphenyltoluene and solid superacid, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of large amount of sulfuric acid, pollution, etc., and achieves simple method, high catalytic reactivity, and reaction The effect of mild conditions

Inactive Publication Date: 2007-07-11
HEILONGJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The purpose of the present invention is to provide a method for preparing 2-nitro-4-thiamphenicol toluene with a solid superacid catalyst in order to solve the problem that the existing p-thiamphenicol toluene nitration process has a large amount of sulfuric acid and serious pollution

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  • Method for preparing 2-nitro-4-methyl p-tolyl sulfone using solid superstrong acid

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specific Embodiment approach 1

[0011] Specific embodiment one: the steps of the method for preparing 2-nitro-4-thiamphenicol toluene in this embodiment are as follows: a, adding to the ice-bath cooled reaction flask with p-thiamphenicol toluene in a molar ratio of 1 to 1.5:1 Concentrated nitric acid, add the solid superacid catalyst of 10%~80% p-thiamphenicol toluene weight again; The reaction temperature is 0-20°C, stir for 20-60 minutes; c, add dropwise an organic solvent containing p-thiamphenicol toluene into the reaction bottle, the reaction temperature is -10-60°C, stir for 2-20 hours, and use high pressure Liquid chromatograph monitors reaction, and when the conversion rate of p-thymphenicol toluene is nearly 100%, stop reaction; d, filter the reaction solution processed through the above steps, and wash the solid with a solvent to obtain a solid superacid catalyst; e, The solution treated in step d is recovered by vacuum distillation to recover the organic solvent; h, the solution distilled in step ...

specific Embodiment approach 2

[0013] Specific embodiment two: In this embodiment, the reaction temperature in step c is 10-40°C. Others are the same as in the first embodiment.

specific Embodiment approach 3

[0014] Specific embodiment three: the organic solvent in step c of this embodiment is dichloromethane, dichloroethane, chloroform or carbon tetrachloride. Others are the same as in the first embodiment.

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Abstract

The invention discloses a making method of 2-nitro-4-thiotoluene catalyzed by solid hyper-strong acid, which comprises the following steps: adding concentrated nitric acid in the ice bath cooling reacting bottle; adding solid hyperstrong acid catalyst; dripping acetic anhydride; stirring 20-60min; dripping organic solvent with p-thiotoluene; stirring 2-10h; filtering to recycle solid hyperstrong catalyst; decompressing; rectifying filtrate; recycling organic solvent; cooling; adding a little of water; filtering; washing solid; drying to obtain the 2-nitro-4-thiotoluene; rectifying the filtrate to recycle acetate.

Description

technical field [0001] The invention relates to a preparation method of nitro compounds, in particular to a method for nitrating 2-nitro-4-thiamphenicol toluene by using solid superacid as a catalyst to catalyze the nitration of p-thiamphenicol toluene. Background technique [0002] 2-nitro-4-thiamphenicol toluene is an important intermediate in organic synthesis, which is used in the production of dyes, medicines and pesticides. Especially as an intermediate of the new high-efficiency cornfield herbicide mesotrione (mesotrion), the demand is constantly increasing. Existing preparation method mostly adopts at present with p-thiamphenicol toluene as raw material, utilizes the method for nitration of mixed acid (US5424481; Fine Chemical Intermediates, 2005,32 (2): 502; Hebei Chemical Industry, 2005, 5: 43-45 ), the disadvantage of this method is that due to the large amount of concentrated sulfuric acid and nitric acid used in the mixed acid nitration process, not only the eq...

Claims

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Application Information

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IPC IPC(8): C07C317/14C07C315/04B01J27/053
CPCY02P20/584
Inventor 孙志忠侯艳君高金胜张彦坤
Owner HEILONGJIANG UNIV