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Preparation method of resorcinol

A technology of phloroglucinol and trimethoxybenzene, which is applied in the field of preparation of phloroglucinol, can solve problems such as post-processing difficulties, and achieve the effects of easy implementation, high product purity, and convenient post-processing

Inactive Publication Date: 2004-07-21
ZHEJIANG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] This method has the following disadvantages: 1. a large amount of concentrated hydrochloric acid has been used, and the ratio of concentrated hydrochloric acid to trimethoxybenzene is 70: 1; 2. in order to neutralize the far excessive concentrated hydrochloric acid, a large amount of Na 2 CO 3 ③The reaction time is as long as 48 hours ④The product is dissolved in a large amount of water, and the post-processing is extremely difficult

Method used

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  • Preparation method of resorcinol
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  • Preparation method of resorcinol

Examples

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preparation example Construction

[0012] The preparation method of phloroglucinol of the present invention is to take 1,3,5-trimethoxybenzene and Lewis acid as raw materials, react in hydrocarbons, halogenated hydrocarbons, aromatic hydrocarbons or substituted aromatic hydrocarbon solvents, and react The temperature is 40-150°C, and then acidic hydrolysis with dilute acid is added. After the acidic hydrolysis is completed, the layers are separated, the water layer is cooled and crystallized, and then recrystallized to obtain phloroglucinol with a content of more than 98.0%.

[0013] The solvent used for the reaction is: hydrocarbons, halogenated hydrocarbons, aromatic hydrocarbons or substituted aromatic hydrocarbon compounds. Hydrocarbons refer to: solvent gasoline, petroleum ether, hexane, cyclohexane, heptane, halogenated hydrocarbons refer to: dichloromethane, chloroform, carbon tetrachloride, dichloroethane, aromatic hydrocarbons or substituted Aromatics refer to: benzene, toluene, xylene, chlorobenzene, ...

Embodiment 1

[0020] Add 300mL of chlorobenzene to a 1000mL three-necked flask equipped with a reflux condenser, dropping funnel, and stirrer, add 0.2mol of trimethoxybenzene and 95.2g (0.7mol) of zinc chloride one by one under stirring, and heat to 120°C. When an intermediate had formed, the reaction was continued for 1 hour and cooled to room temperature. Add dropwise 500mL of 2NHCl acidolysis intermediate therein, after acidolysis is complete, separate layers, cool and crystallize the water layer, and filter to obtain crude phloroglucinol, which is recrystallized with water and dried to obtain 22.8g of phloroglucinol finished product (content 98.7% ), yield 89.3%.

Embodiment 2～ Embodiment 9

[0022] Change the type or amount of Lewis acid, others are the same as in Example 1, and the results are shown in Table 1

[0023] Example

[0024]

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Abstract

jA process for preparing phloroglucinol from 1,3,5-trimethoxy benzene includes reacting on lewis acid in the hydrocarbon-type solvent to generate intermediate, acidic hydrolyzing by inorganic acid, layering, crystallizing in liquid layer, and recrystallizing. Its advantages are short time, high productivity and high purity and output rate of product.

Description

technical field [0001] The invention relates to a preparation method of phloroglucinol. Background technique [0002] Before the present invention, the method reported in literature [Zhu Aishi, Xu Huaxin, chemical process and technology, 17 (25), 128~132 (2001)] is to use concentrated hydrochloric acid as ether bond breaking reagent, and its reaction formula is as follows : [0003] [0004] This method has the following disadvantages: 1. a large amount of concentrated hydrochloric acid has been used, and the ratio of concentrated hydrochloric acid to trimethoxybenzene is 70: 1; 2. in order to neutralize the far excessive concentrated hydrochloric acid, a large amount of Na 2 CO 3 ③The reaction time is as long as 48 hours. ④The product is dissolved in a large amount of water, and post-processing is extremely difficult. Contents of the invention [0005] The purpose of this invention is to provide a kind of prepa...

Claims

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Application Information

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IPC IPC(8): C07C37/055C07C39/10
Inventor 黄国东陈志荣
Owner ZHEJIANG UNIV
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