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3-hydroxyacetophenone synthesis method

A technology for hydroxyacetophenone and a synthesis method, which is applied in the preparation of carbon-based compounds, chemical instruments and methods, and preparation of carbonyl compounds by condensation, etc., can solve the problems of large amount of sewage, serious environmental pollution and low yield in the production process.

Active Publication Date: 2016-09-28
BEIJING RISUN TECH CO LTD
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Problems solved by technology

[0010] Aiming at the problems of large amount of sewage, serious environmental pollution, low yield and potential safety hazards in the production process in the existing 3-hydroxyacetophenone production process, the inventors conducted extensive and in-depth research and finally obtained the present invention
The synthesis method of 3-hydroxyacetophenone of the present invention can solve the problems of large amount of sewage, serious environmental pollution, low yield and potential safety hazards in the production process of 3-hydroxyacetophenone in the existing production process

Method used

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Embodiment 1

[0057]

[0058] Step (1): Add 50g of 3-hydroxybenzoic acid, 67g of acetic anhydride and 0.35g of concentrated sulfuric acid to the reaction vessel, heat up to 100°C under stirring and react for 30 minutes. After the reaction is over, distill under reduced pressure Removal of the solvent gave 64.5 g of 3-acetoxybenzoic acid (crude) as a white solid.

[0059] Step (2): Add 50 g of 3-acetoxybenzoic acid and 725 ml of toluene as a reaction solvent to the reaction vessel, then slowly add 56 g of thionyl chloride dropwise to the reaction system, and after the dropwise addition, heat up to the solvent After reacting at 100°C for 1 h, the solvent and unreacted thionyl chloride were removed by vacuum distillation to obtain 70.3 g of 3-acetoxybenzoyl chloride with a yield of 98% (crude product).

[0060] Step (3): Add 62.2 g of dimethyl malonate and 34.4 g of magnesium chloride to 600 ml of dichloromethane, slowly add triethylamine dropwise at an internal temperature of 5°C, and star...

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Abstract

The invention provides a 3-hydroxyacetophenone synthesis method. The method includes the steps that 3-hydroxybenzoic acid is subjected to hydroxyl protection through an esterification or etherification reaction, then a chloroformylation reaction and an alkylation reaction are conducted, finally hydrolysis is conducted, and the 3-hydroxyacetophenone is obtained. According to the method, raw materials are cheap, easy to obtain and wide in source, high-temperature and high-pressure operation does not exist, equipment requirement is low, and equipment investment is low; peroxide, heavy nitride and the like do not exist, and high safety is achieved; compared with a nitration-iron powder reduction-diazotization route commonly adopted in the nation, the synthesis method has huge environment-friendly advantages. Besides, according to the method, the amount of wastewater is less than 5% that of an original process, the total route yield is 90%, and the method has huge technological advantages.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a synthesis method of 3-hydroxyacetophenone. Background technique [0002] 3-Hydroxyacetophenone, also known as m-hydroxyacetophenone, m-hydroxyacetophenone, 3-hydroxyacetophenone, 3-acetylphenol, m-acetylphenol, 3-hydroxyacetylketone, etc., is the synthesis of phenylephrine Intermediates are in great demand in the market. The chemical structure of 3-hydroxyacetophenone is shown below: [0003] [0004] At present, the main synthetic methods of 3-hydroxyacetophenone include the following: [0005] 1) The process route generally adopted by enterprises is to use acetophenone as the starting material, and to obtain m-nitroacetophenone through meta-nitration with mixed acid under the condition of -10~0°C, and crystallize and separate in ice water to obtain m-nitrobenzene Crude ethyl ketone, add the crude product to iron powder and hydrochloric acid system for reduc...

Claims

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Application Information

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IPC IPC(8): C07C45/65C07C49/825
CPCC07C45/45C07C45/65C07C51/367C07C51/60C07C65/21C07C49/84C07C49/825
Inventor 张英伟胡滨杨学林王鹏慧谢增勇
Owner BEIJING RISUN TECH CO LTD
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