2-methyl-3-methoxybenzoyl chloride synthesizing process

A technology of methoxybenzoyl chloride and methoxybenzoic acid, which is applied in the field of synthesis of 2-methyl-3-methoxybenzoyl chloride, can solve the problems of high preparation cost and low yield, and achieve Low cost, stable and reliable product quality

Inactive Publication Date: 2019-02-26
JIANGSU YONGAN CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Purpose of the invention: the purpose of the present invention is to provide a kind of 2-methyl-3-methoxybenzoyl chloride in order to solve the problem of high preparation cost and low yield of 2-methyl-3-methoxybenzoyl chloride in the prior art. The preparation technology of phenylbenzoyl chloride

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] The synthesis technique of 2-methyl-3-methoxybenzoyl chloride comprises the following steps connected in sequence:

[0023] 1) Preparation of 3-nitro-o-xylene: use o-xylene as raw material to obtain 3-nitro-o-xylene through nitration reaction, specifically, use o-xylene as raw material to cool to -10°C, drop under stirring conditions Add pre-cooled mixed acid, the dropping temperature is -10°C, continue to stir for 0.5 hours after the dropping is completed, let stand to separate the lower layer of waste acid, take the upper layer of nitration solution and wash it with water, 5% sodium hydroxide solution and water successively, and then carry out Steam distillation and further fractionation obtain 3-nitro-o-xylene; the mixed acid is made of 1 part by weight of 66% nitric acid and 2 parts of 98% sulfuric acid, 95g of o-xylene, and 245g of mixed acid.

[0024] 2) Preparation of 2-methyl-3-nitrobenzoic acid: In a high-pressure oxidation reactor with a reflux device, put 100...

Embodiment 2

[0035] The synthesis technique of 2-methyl-3-methoxybenzoyl chloride comprises the following steps connected in sequence:

[0036] 1) Preparation of 3-nitro-o-xylene: use o-xylene as raw material to obtain 3-nitro-o-xylene through nitration reaction, specifically, use o-xylene as raw material to cool to -12°C, drop under stirring conditions Add pre-cooled mixed acid, the dropping temperature is -12°C, continue to stir for 0.5 hours after the dropping is completed, let stand to separate the lower layer of waste acid, take the upper layer of nitration solution and wash it with water, 5% sodium hydroxide solution and water successively, and then carry out Steam distillation and further fractionation obtain 3-nitro-o-xylene; the mixed acid is made of 1 part by weight of 65% nitric acid and 2 parts of 97.5% sulfuric acid, 190 g of ortho-xylene, and 490 g of mixed acid.

[0037] 2) Preparation of 2-methyl-3-nitrobenzoic acid: In a high-pressure oxidation reactor with a reflux device...

Embodiment 3

[0048] The synthesis technique of 2-methyl-3-methoxybenzoyl chloride comprises the following steps connected in sequence:

[0049] 1) Preparation of 3-nitro-o-xylene: use o-xylene as raw material to obtain 3-nitro-o-xylene through nitration reaction, specifically, use o-xylene as raw material to cool to -8°C, drop under stirring conditions Add pre-cooled mixed acid, the dropping temperature is -8°C, continue to stir for 0.3 hours after the dropping is completed, let stand to separate the lower layer of waste acid, take the upper layer of nitration solution and wash it with water, 4% sodium hydroxide solution and water successively, and then carry out Steam distillation and further fractionation obtain 3-nitro-o-xylene; the mixed acid is made of 1.1 parts by weight of 66% nitric acid and 2 parts of 96% sulfuric acid, 90 g of o-xylene, and 232 g of mixed acid.

[0050] 2) Preparation of 2-methyl-3-nitrobenzoic acid: In a high-pressure oxidation reactor with a reflux device, put ...

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PUM

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Abstract

The invention discloses a 2-methyl-3-methoxybenzoyl chloride synthesizing process. According to the present invention, low-cost o-xylene is used as a starting raw material, the product is synthesizedby using a conventional synthesis method comprising nitrification, esterification, reduction, diazotization, methylation, acyl chlorination and other steps, and the total yield is controlled at more than 65%; the esterification of the intermediate product improves the separation degree of the intermediate; the reaction solvent is added in the diazotization step, such that the process parameters are relatively easy to control, and the purity of the intermediate in the diazotization step is more than 96% so as to provide the guarantee for the quality of the subsequent product; and with the synthesis process, the product quality is stable and reliable, and the cost is low.

Description

technical field [0001] The invention belongs to the field of synthesis technology of organic intermediates, in particular to a synthesis technology of 2-methyl-3-methoxybenzoyl chloride. Background technique [0002] Methoxyfenozide is a second-generation dihydrazide insect growth regulator and an ecdysone insecticide, which interferes with the normal growth and development of insects and inhibits feeding. It is mainly used in vegetables and farmland to control vegetables (melons, solanaceous fruits), apples, corn, cotton, grapes, kiwi, walnuts, flowers, sugar beets, tea and field crops (rice, sorghum, soybeans) and other crops. Lepidoptera pests. Especially effective on larvae and eggs. It is safe to beneficial insects and beneficial mites, and has activities such as contact killing and root systemic absorption. Friendly to the environment. 2-Methyl-3-methoxybenzoyl chloride is an important intermediate of the pesticide methoxyfenozide, so it is of great significance to...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/60C07C65/21
CPCC07C51/09C07C51/60C07C67/31C07C201/08C07C201/12C07C227/04C07C205/06C07C205/57C07C229/60C07C69/84C07C69/92C07C65/21
Inventor 沈亮明王晓军陈湘朋吴浩陈夕鹏
Owner JIANGSU YONGAN CHEM CO LTD
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