M-hydroxy acetophenone preparation method

A technology of m-hydroxyacetophenone and hydroxyacetophenone, which is applied in the field of preparation of m-hydroxyacetophenone, can solve the problems of large waste water discharge, high environmental protection cost, and high cost, and achieve small waste water discharge, avoid pollution, low cost effect

Inactive Publication Date: 2018-09-14
JIANGXI YONGTONG TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, the traditional process has a large amount of waste water discharge, and the waste water discharge per ton of product reaches 30 tons, which makes the cost of environmental protection large and high.

Method used

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  • M-hydroxy acetophenone preparation method

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Experimental program
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Effect test

Embodiment 1

[0031] A preparation method of m-hydroxyacetophenone, which comprises the following steps:

[0032] (1) Chlorination, dissolve meta-hydroxybenzoic acid in toluene, add 4-dimethylaminopyridine as a catalyst, and then add thionyl chloride for chlorination to obtain meta-hydroxybenzoic acid chloride, which is then concentrated and evaporated. Remove thionyl chloride to obtain m-hydroxybenzoic acid chloride-toluene solution;

[0033] (2) Dissolve dimethyl malonate sodium salt in toluene to obtain dimethyl malonate sodium salt-toluene solution, and then add the m-hydroxybenzoic acid chloride-toluene solution obtained in step (1) dropwise to the malonate Dimethyl acid sodium salt-toluene solution, and then react, and reflux reaction is performed at a reaction temperature of 60°C for 4 hours to obtain product A;

[0034] (3) Add the product A obtained in step (2) to a hydrochloric acid solution, and perform a hydrolysis reaction to obtain m-hydroxyacetophenone.

[0035] In the step (1) the ...

Embodiment 2

[0040] A preparation method of m-hydroxyacetophenone, which comprises the following steps:

[0041] (1) Chlorination, dissolve meta-hydroxybenzoic acid in toluene, add 4-dimethylaminopyridine as a catalyst, and then add thionyl chloride for chlorination to obtain meta-hydroxybenzoic acid chloride, which is then concentrated and evaporated. Remove thionyl chloride to obtain m-hydroxybenzoic acid chloride-toluene solution;

[0042] (2) Dissolve dimethyl malonate sodium salt in toluene to obtain dimethyl malonate sodium salt-toluene solution, and then add the m-hydroxybenzoic acid chloride-toluene solution obtained in step (1) dropwise to the malonate In the dimethyl acid sodium salt-toluene solution, the reaction is carried out, and the reflux reaction is carried out at a reaction temperature of 70° C. for 4 hours to obtain product A;

[0043] (3) Add the product A obtained in step (2) to a hydrochloric acid solution, and perform a hydrolysis reaction to obtain m-hydroxyacetophenone. ...

Embodiment 3

[0049] A preparation method of m-hydroxyacetophenone, which comprises the following steps:

[0050] (1) Chlorination, dissolve meta-hydroxybenzoic acid in toluene, add 4-dimethylaminopyridine as a catalyst, and then add thionyl chloride for chlorination to obtain meta-hydroxybenzoic acid chloride, which is then concentrated and evaporated. Remove thionyl chloride to obtain m-hydroxybenzoic acid chloride-toluene solution;

[0051] (2) Dissolve dimethyl malonate sodium salt in toluene to obtain dimethyl malonate sodium salt-toluene solution, and then add the m-hydroxybenzoic acid chloride-toluene solution obtained in step (1) dropwise to the malonate In the dimethyl acid sodium salt-toluene solution, the reaction is carried out, and the reflux reaction is carried out at a reaction temperature of 75°C for 4.2 hours to obtain product A;

[0052] (3) Add the product A obtained in step (2) to a hydrochloric acid solution, and perform a hydrolysis reaction to obtain m-hydroxyacetophenone. ...

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Abstract

The invention discloses an m-hydroxy acetophenone preparation method which includes the steps: performing chlorination, dissolving m-hydroxybenzoic acid in methylbenzene, adding 4-dimethylamino pyridine serving as a catalyst, adding acyl thionyl chloride for chlorination to obtain m-hydroxybenzoic acid acyl chloride, and then removing the acyl thionyl chloride by concentration and evaporation to obtain m-hydroxybenzoic acid acyl chloride-methylbenzene solution; dissolving dimethyl malonate sodium salt in methylbenzene to obtain dimethyl malonate sodium salt-methylbenzene solution, dripping them-hydroxybenzoic acid acyl chloride-methylbenzene solution obtained in the step (1) into the dimethyl malonate sodium salt-methylbenzene solution, and then performing reflux reaction for 3-5 hours atthe reaction temperature of 50-80 DEG C to obtain a product A; adding the obtained product A into hydrochloric acid solution, and performing hydrolysis reaction to obtain m-hydroxy acetophenone. Thepreparation method is simple in process, small in wastewater discharge amount, low in cost and high in yield and final product purity.

Description

Technical field [0001] The invention relates to a preparation method of m-hydroxyacetophenone, belonging to the technical field of organic synthesis. Background technique [0002] M-hydroxyacetophenone is a needle-like crystal. The melting point is 95-97°C, the boiling point is 296°C, 153°C (0.67kPa), the relative density is 1.099 (109°C), and the refractive index is 1.5348. Soluble in ethanol; ether; chloroform and benzene, slightly soluble in water, insoluble in petroleum ether. Used in organic synthesis, it is an intermediate of the drug phenylephrine. [0003] The conventional production method is derived from the reaction between m-aminoacetophenone and sodium nitrite. Add water and sulfuric acid into the reaction pot, add m-aminoacetophenone under stirring, then add dropwise sodium nitrite aqueous solution under cooling, keep the temperature at 8-10℃, slowly increase the temperature to above 90℃ after the addition, continue stirring the reaction 1h. The solid is precipit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/42C07C49/825
CPCC07C45/42C07C51/60C07C67/313C07C49/825C07C65/03C07C69/738
Inventor 刘忠春
Owner JIANGXI YONGTONG TECH
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