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Preparation method of 2-(4-ethoxyphenyl)-2.2-dimethylethanol

A technology of ethoxyphenyl and dimethyl ethanol, which is applied in the field of pesticides, can solve the problems of high price, complex process, and low cost, and achieve the effects of low product cost, reasonable process, and high safety

Inactive Publication Date: 2018-08-07
LIANYUNGANG GUOSHENG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It has the advantages of low product cost, high quality, environmental friendliness, and is more suitable for industrial production, and solves the problems of complex, expensive and toxic existing processes

Method used

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  • Preparation method of 2-(4-ethoxyphenyl)-2.2-dimethylethanol
  • Preparation method of 2-(4-ethoxyphenyl)-2.2-dimethylethanol
  • Preparation method of 2-(4-ethoxyphenyl)-2.2-dimethylethanol

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preparation example Construction

[0027] A preparation method of 2-(4-ethoxyphenyl)-2.2-dimethylethanol, the preparation steps are as follows:

[0028] Take 1 mole of acid and dissolve it in 300-600ml of alcohol solvent, or in a mixed solvent composed of alcohol solvent and ether solvent, the alcohol solvent is methanol or ethanol, and the ether solvent is selected from tetrahydrofuran, 2-methyltetrahydrofuran , dioxane, diethyl ether, isopropyl ether or methyl tert-butyl ether; the acid is:

[0029]

[0030] Raise the temperature to 30-85°C; add borohydride and metal salt, the molar ratio of borohydride, metal salt to substrate is 1.1-2.0:0.55-1.0:1.0; continue to keep warm for 3-8 hours; recover alcohol under reduced pressure Mixed solvent composed of solvent or alcohol solvent and ether solvent; add 300-600ml of organic solvent, stir and drop hydrochloric acid until the pH value of the reaction material is 3-4, then add 200-500ml of water, stand still, and extract by layers. The organic solvent is selec...

Embodiment 1

[0035] Take 1 mole of acid and dissolve it in 300-600ml of alcohol solvent, or in a mixed solvent composed of alcohol solvent and ether solvent, the alcohol solvent is methanol or ethanol, and the ether solvent is selected from tetrahydrofuran, 2-methyltetrahydrofuran , dioxane, diethyl ether, isopropyl ether or methyl tert-butyl ether; the acid is:

[0036]

[0037] Raise the temperature to 30°C; add borohydride and metal salt, the molar ratio of borohydride, metal salt and substrate is 1.5:0.5:1; continue to keep warm for 3 hours; recover alcohol solvent or alcohol and ether solvent under reduced pressure A mixed solvent composed of: add 300-600ml of organic solvent, stir and drop hydrochloric acid until the pH value of the reaction material is 3-4, then add 200-500ml of water, the organic solvent is selected from ethyl acetate, dichloromethane, Chloroform or dichloroethane, toluene; dry the organic phase with anhydrous sodium sulfate, and concentrate under reduced pressu...

Embodiment 2

[0039] Take 1 mole of acid and dissolve it in 300-600ml of alcohol solvent, or in a mixed solvent composed of alcohol solvent and ether solvent, the alcohol solvent is methanol or ethanol, and the ether solvent is selected from tetrahydrofuran, 2-methyltetrahydrofuran , dioxane, diethyl ether, isopropyl ether or methyl tert-butyl ether; the acid is:

[0040]

[0041] Raise the temperature to 85°C; add borohydride and metal salt, the molar ratio of borohydride, metal salt and substrate is 2.0:1.5:1; continue to keep warm for 8 hours; recover alcohol solvent or alcohol solvent and ether solvent under reduced pressure A mixed solvent composed of: add 300-600ml of organic solvent, stir and drop hydrochloric acid until the pH value of the reaction material is 3-4, then add 200-500ml of water, the organic solvent is selected from ethyl acetate, dichloromethane, Chloroform or dichloroethane, toluene; dry the organic phase with anhydrous sodium sulfate, and concentrate under reduce...

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Abstract

The invention discloses a preparation method of 2-(4-ethoxyphenyl)-2.2-dimethylethanol. The preparation method comprises the following preparation steps: (1) dissolving one mole of acid in an alcoholsolvent, or in a mixed solvent consisting of the alcohol solvent and an ethers solvent; (2) heating the mixed solvent in step (1); and adding borohydride and metal salt; (3) continuing carrying out heat-insulation reaction, and recycling the alcohol solvent or the alcohol solvent or the ethers solvent under reduced pressure; and adding an organic solvent, dropwise adding hydrochloric acid while stirring to react, adding the organic solvent again, standing, layering and extracting; and drying an organic phase by using anhydrous sodium sulfate, and concentrating under reduced pressure to obtainthe product. Compared with the prior art, the method is high in safety, and the process is reasonable, simple and conveniently; and raw materials are easily obtained. The cost of the product is low, the quality is high, and the preparation method is environmentally friendly, and is suitable for industrial production; and the total yield of reaction taking 2-(4-ethoxyphenyl)-2.2-dimethylacetic acidcan reach 95% or above, and the content of the product reaches 98%.

Description

technical field [0001] The invention relates to the technical field of pesticides, in particular to a preparation method of 2-(4-ethoxyphenyl)-2.2-dimethylethanol. Background technique [0002] 2-(4-Ethoxybenzene)-2-methylpropanol is the raw material for the synthesis of Etofenprox, Etofenprox (common name: etofenprox, trade name: Trebon) is also known as Doraemon, Resmethrin, Lilaiduo and Yifenning are high-efficiency pyrethroid insecticides discovered by Mitsui Toatsu Chemicals Inc. in Japan in the early 1980s. They have a wide insecticidal spectrum, high insecticidal activity, and knock down It is fast, long-lasting, and safe for crops. It is used to control Lepidoptera, Hemiptera, Diptera and Isoptera pests, such as brown planthopper, white-backed planthopper, black-tailed leafhopper, cotton bollworm, Pink bollworm, green peach aphid, melon aphid, whitefly, cabbage caterpillar, tea caterpillar, tea ruler, tea thorn moth, peach and pear small borer, citrus leaf miner, to...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/26C07C43/23
CPCC07C41/26C07C43/23
Inventor 徐晨朱国庆张鑫周土林
Owner LIANYUNGANG GUOSHENG CHEM