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Synthetic method of 2-chloro-4-aminophenol

A synthesis method and aminophenol technology are used in the synthesis of pesticide intermediates, and in the field of synthesis of 2-chloro-4-aminophenol, which can solve reaction difficulties, low yield of 2-chloro-4-aminophenol, and low yield of 2-chloro-4-aminophenol. There are many problems such as by-products and large pollution, so as to achieve the effect of saving synthesis cost, high purity and low pollution

Active Publication Date: 2014-12-10
安徽宁亿泰科技有限公司
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  • Application Information

AI Technical Summary

Problems solved by technology

[0021] The purpose of the present invention is to overcome defects such as low yield, difficult reaction, and large pollution of by-products in the existing synthesis of 2-chloro-4-aminophenol, thereby providing a high-yield, safe and easy-to-operate synthetic 2-chlorophenol - the method of 4-aminophenol; the method has short synthetic route, high yield, high product content, low cost, and meets the requirements of large-scale safe production

Method used

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  • Synthetic method of 2-chloro-4-aminophenol

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Embodiment l

[0040] The synthesis of embodiment 1,2-chloro-4-nitrophenol

[0041] Add 60 grams of 99% p-nitrophenol (0.427 moles) and 240 grams of solvent dichloroethane in a 500 milliliter four-necked bottle equipped with a thermometer, agitator, reflux condenser and tail gas absorption device, stir and heat to 55-65°C, open the vacuum tail gas absorption system to ensure that the condition is slightly negative -0.01-0.02MPa, then pass chlorine gas, use GC to track the reaction process, and wait for the reaction of raw materials to complete. Firstly, recover the solvent dichloroethane from atmospheric pressure precipitation and apply it directly, and then distill the residual solvent dichloroethane under reduced pressure at 10mmHg to recover the cover steam to obtain the crude product o-chloro-p-nitrophenol, lower the temperature to below 50°C, add 200 grams of toluene, and heat up After complete dissolution, slowly cool down to natural precipitation, then cool down in an ice bath to (0-5...

Embodiment 2

[0042] The synthesis of embodiment 2,2-chloro-4-aminophenol

[0043] Add 107 grams of o-chloro-p-nitrophenol (0.62 moles) and 210 grams of water, 4.9 grams of activated carbon and 1.2 grams of Ferric chloride hexahydrate, add 12.4 grams of 30% sodium hydroxide (0.093 moles) solution dropwise. Let the temperature rise naturally, and the drop will be completed in about 30 minutes. Make the raw material fully contact with the catalyst. Add 128 grams of 40% hydrazine hydrate (1.023 moles) dropwise at 95-100°C, keep the temperature for 3 hours after dropping, after the reaction is completed, the reaction solution is cooled to 40-45°C and filtered, and the filter residues are washed twice with 100 ml of water, combined After the filtrate, 30% concentrated hydrochloric acid was added dropwise until neutral, and the precipitated light yellow solid was filtered and dried to obtain 85.0 g of 2-chloro-4-aminophenol, with a qualitative content of 98.2% and a qualitative yield of 93.8%. ...

Embodiment 3

[0044] Embodiment 3, catalyst recovery is used for the synthesis of 2-chloro-4-aminophenol

[0045] Add 107 grams of o-chloro-p-nitrophenol (0.62 mole), 210 grams of water, 5.3 grams of reclaimed catalyst (activated carbon and six After stirring, add 10.7 grams of 30% sodium hydroxide (0.080 mol) solution dropwise. After about 30 minutes, the temperature is raised to 95-100°C and kept at this temperature for 0.5 hours, so that the raw materials and Catalyst full contact. Add 128 grams of 40% hydrazine hydrate (1.023 moles) dropwise at 95-100°C, and keep the temperature for 3 hours after dropping. After the reaction is completed, the reaction solution is cooled to 40-45°C and filtered, and the filter residues are washed twice with 100 ml of water. After combining the filtrates, 30% concentrated hydrochloric acid was added dropwise until neutral, and the precipitated light yellow solid was filtered and dried to obtain 84 grams of 2-chloro-4-aminophenol, with a qualitative conte...

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Abstract

The invention discloses a synthetic method of 2-chloro-4-aminophenol. The synthetic method comprises the following steps: obtaining the 2-chloro-4-nitrophenol by carrying out a chlorination reaction on nitrophenol and chlorine in inertia organic solvent; and firstly adding sodium hydroxide into the 2-chlorine-4-nitrophenol under the existence of a catalytic agent such as activated carbon and ferric trichloride hexahydrate, and then slowly adding hydrazine hydrate to carry out a reduction reaction so as to synthesize the 2-chloro-4-aminophenol. The catalytic agent in the synthetic method of the 2-chloro-4-aminophenol can be recycled and used mechanically for at least ten times. Therefore, the synthetic method of the 2-chlorine-4-aminophenol has the advantages of being high in yield, high in purity, less in environmental pollution and extremely strong in market competitiveness.

Description

technical field [0001] The invention relates to a synthesis method of an insecticide intermediate, in particular to a new synthesis method of 2-chloro-4-aminophenol, which belongs to the field of synthesis of insect growth regulator fenfluramide. Background technique [0002] 2-Chloro-4-aminophenol is the main intermediate in the synthesis of benzoylurea insecticide difenfluramide. Difenfluramide is a new type of insect growth regulator. Its mechanism of action is to inhibit the synthesis of chitin in pests, so that pests cannot form new epidermis when moulting, and the insects are deformed and die. At the same time, it can also regulate the growth and development of insects. , Inhibit molting metamorphosis, inhibit the feeding speed of pests, have strong knockdown power and high ovicidal activity, especially have good control effects on pests resistant to pyrethroids and organophosphorus pesticides. The insecticide has excellent properties such as broad-spectrum high effic...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C215/76C07C213/02
CPCY02P20/584
Inventor 王凤云王正旭张胜吴耀军
Owner 安徽宁亿泰科技有限公司
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