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Preparation method of phenylacetic acid type compound

The technology of a compound and phenylacetic acid, applied in the field of preparation of phenylacetic acid compounds, can solve the problems of large amount of catalyst, toxic three wastes, complicated operation, etc., and achieve the effects of reducing the overall usage amount, reducing the reaction pressure, and being easy to obtain.

Active Publication Date: 2019-02-12
JIANGSU LIANHE CHEM TECH +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] The technical problem to be solved by the present invention is to overcome the existing toxic material sodium cyanide used in the cyanation method when preparing phenylacetic acid compounds, which causes the generation of toxic wastes and safety risks; , there are defects such as large amount of catalyst used, high pressure, cumbersome operation, etc., and a mixed catalyst using cheap pyridine-2-carboxylate cobalt and palladium acetate is provided, which can obtain the preparation of phenylacetic acid compounds simply and efficiently method

Method used

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  • Preparation method of phenylacetic acid type compound
  • Preparation method of phenylacetic acid type compound
  • Preparation method of phenylacetic acid type compound

Examples

Experimental program
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Effect test

Embodiment 1

[0039]

[0040] Add 64.4g (0.4mol) of p-chlorobenzyl chloride, add 0.55g of cobalt pyridine-2-carboxylate, 1.37g of palladium acetate, add 160g (1.2mol) of 30% NaOH, 73.7g of methanol (1.6mol) and replace the system with CO three times , heated up to 150°C, charged with CO until the pressure in the kettle was 1.5MPa, kept the temperature for 5hrs, cooled to room temperature, distilled under reduced pressure to remove methanol, filtered off the catalyst, added 30% hydrochloric acid to adjust the pH to 1, filtered, and dried to obtain p-chloro Phenylacetic acid, the purity is: 99.76%, the yield is 85%.

Embodiment 2

[0042]Add 64.4g (0.4mol) of p-chlorobenzyl chloride, add 0.55g of cobalt pyridine-2-carboxylate, 1.37g of palladium acetate, add 121g (1.2mol) of triethylamine, 73.7g of methanol (1.6mol) and replace the system with CO 3 times , heat up to 150°C, pour in CO until the pressure in the kettle is 1.5MPa, keep the temperature for 5hrs, cool down to room temperature, remove methanol and part of triethylamine by distillation under reduced pressure, filter out the catalyst, add 30% hydrochloric acid to adjust the pH to 1, filter , drying to obtain p-chlorophenylacetic acid with a purity of 99.25% and a yield of 80%.

Embodiment 3

[0044] Add 64.4g (0.4mol) of p-chlorobenzyl chloride, add 0.773g of cobalt pyridine-2-carboxylate, 1.16g of palladium acetate, add 160g (1.2mol) of 30% NaOH, 73.7g of methanol (1.6mol) and replace the system with CO three times , heated up to 150°C, charged with CO until the pressure in the kettle was 1.5MPa, kept the temperature for 5hrs, cooled to room temperature, distilled under reduced pressure to remove methanol, filtered off the catalyst, added 30% hydrochloric acid to adjust the pH to 1, filtered, and dried to obtain p-chloro Phenylacetic acid, the purity is: 99.29%, the yield is 82%.

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Abstract

The invention discloses a preparation method of a phenylacetic acid type compound. The preparation method of the phenylacetic acid type compound I comprises the following steps that in a solvent and aCO gas phase system, a benzyl halide type compound II, pyridine-2-cobalt carboxylate, palladium acetate and alkaline neutralizers take carbonylation reaction to obtain the phenylacetic acid type compound I. A mixed catalytic system has a synergistic effect; the whole use quantity of catalysts is greatly reduced. When the mixed catalyst is used, a better catalytic effect can be achieved; the characteristics of easily obtaining the catalyst, avoiding the production safety risk of toxic three wastes and the like, reducing the reaction pressure, realizing mild reaction conditions, reducing the production risk, facilitating the production and the like are realized. The formulas are shown in description.

Description

technical field [0001] The invention relates to a preparation method of phenylacetic acid compounds. Background technique [0002] Phenylacetic acid compounds are important fine chemical intermediates, widely used in medicine, pesticides, spices, dyes and other fields. [0003] For example, p-chlorophenylacetic acid is an intermediate in organic synthesis of medicines, pesticides, spices, etc. In industrial production, it is widely used in S-fenvalerate, 6-chloro-3,4-dihydro-1H-2-naphthalenone, pyrethrin, 4-chlorophenylethanol, fenvalerate, and bromide Production of downstream products such as permethrin. [0004] There are two synthesis methods of phenylacetic acid derivatives reported so far: benzyl chloride cyanation method and benzyl chloride carbonylation method. [0005] The cyanation method is reported in the patent CN102757337A, using o-chlorobenzyl chloride as the starting material, one-pot method to prepare o-chlorophenylacetic acid, mixing o-chlorobenzyl and tr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C57/58C07C57/30C07C59/64C07C51/10C07C205/56C07C201/12C07C255/57C07C253/30
CPCC07C51/10C07C201/12C07C253/30C07C57/58C07C57/30C07C59/64C07C205/56C07C255/57
Inventor 王辉何朝晖徐晓明
Owner JIANGSU LIANHE CHEM TECH
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