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Preparation method of 2,4,6-trimethylbenzaldehyde

A technology of trimethylbenzaldehyde and trimethylbenzene, which is applied in the field of agricultural chemical raw materials, can solve the problems of unreported yield, long reaction time, and high equipment requirements, and achieve easy removal, low equipment requirements, and low catalyst cost Effect

Active Publication Date: 2018-07-20
HEBEI UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0012] Fergus et al. used the formylating reagent N, N-dimethylformamide, and reacted overnight at room temperature after adding the reagent dropwise at -78°C under catalyst-free conditions. The yield of the reaction was not reported, and the method required a very low temperature. High requirements on equipment, long response time, increased cost

Method used

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  • Preparation method of 2,4,6-trimethylbenzaldehyde
  • Preparation method of 2,4,6-trimethylbenzaldehyde
  • Preparation method of 2,4,6-trimethylbenzaldehyde

Examples

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Embodiment 1

[0032] Add 43.8g (0.6mol) N,N-dimethylformamide and 150mL anhydrous dichloromethane into the reaction flask, slowly add 30.6g (0.2mol) POCl 3 After stirring at -10°C for 20min, 12.0g (0.1mol) of 2,4,6-trimethylbenzene was added dropwise, the temperature was controlled below -5°C and stirred for 10min, and the reaction was refluxed for 6.0h. Post-treatment process: remove dichloromethane under reduced pressure, slowly pour into 450 mL of ice water, neutralize the mixed solution with saturated sodium carbonate to pH = 7, then extract three times with 100 mL of ethyl acetate, combine the organic layers, dry, and desolventize to obtain Liquid 2,4,6-trimethylbenzaldehyde 13.4g, content 95.0%, yield 90.3%.

Embodiment 2

[0034] Add 43.8g (0.6mol) N,N-dimethylformamide and 150mL anhydrous chloroform into the reaction flask, slowly add 30.6g (0.2mol) POCl 3 After stirring at -10°C for 20min, 12.0g (0.1mol) of 2,4,6-trimethylbenzene was added dropwise, the temperature was controlled below -5°C and stirred for 10min, and the reaction was refluxed for 6.0h. Post-treatment process: remove chloroform under reduced pressure, slowly pour into 450 mL of ice water, neutralize the mixed solution with saturated sodium carbonate to pH = 7, then extract three times with 100 mL of ethyl acetate, combine the organic layers, dry, and desolventize to obtain Liquid 2,4,6-trimethylbenzaldehyde 11.3g, content 90.0%, yield 76.2%.

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Abstract

The invention discloses a preparation method of intermediate 2,4,6-trimethylbenzaldehyde of herbicide tralkoxydim and belongs to the technical field of agricultural chemical materials. The method comprises the steps as follows: N,N-dimethylformamide and an anhydrous organic solvent are added to a reaction bottle, a certain amount of POCl3 is slowly dropwise added, stirring is performed at subzero10 DEG C for 20 min, 2,4,6-trimethylbenzene is dropwise added, stirring is performed at the temperature of subzero 5 DEG C for 10 min, a reflux reaction is conducted for 4.0-8.0 h, after the reaction,the organic solvent is removed under reduced pressure, a certain amount of ice water is slowly added, the mixed solution is neutralized with saturated sodium carbonate until the pH is 7, extraction is performed multiple times with ethyl acetate, organic layers are mixed, and 2,4,6-trimethylbenzaldehyde (I) is obtained after drying and desolvation.

Description

technical field [0001] The present invention relates to a preparation method of the intermediate 2,4,6-trimethylbenzaldehyde of the cyclohexanedione herbicide trimethylbenzalone, and specifically involves using 2,4,6-trimethylbenzene as a raw material The invention discloses a method for preparing 2,4,6-trimethylbenzaldehyde in the next step under the conditions of an organic solvent and a catalyst, which belongs to the technical field of agricultural chemical raw materials. Background technique [0002] 2,4,6-Trimethylbenzaldehyde, commonly known as rice aldehyde, is a colorless or light yellow liquid with a melting point of 14°C and is stable at room temperature. As an important intermediate, it is widely used in pesticides, pharmaceuticals and resin additives, and is one of the high value-added fine chemicals. Due to the hindrance of three methyl groups in its molecular structure, its preparation method has always attracted attention. [0003] For example, the Gartman-K...

Claims

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Application Information

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IPC IPC(8): C07C45/45C07C47/542
CPCC07C45/455C07C47/542
Inventor 李婉杨子辉武世杰
Owner HEBEI UNIVERSITY