Synthetic method for 3,4-dihydroxybenzaldehyde
A technology of dihydroxybenzaldehyde and hydroxybenzaldehyde, which is applied in the field of synthesis of 3,4-dihydroxybenzaldehyde, can solve the problems of toxic raw materials and cumbersome steps, and achieve simple and easy operation, low cost and shortened reaction route Effect
Inactive Publication Date: 2020-01-03
胡婷
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Problems solved by technology
[0003] The purpose of the present invention is to solve the problems of cumbersome steps and toxic raw materials in the existing traditional synthetic method, and provide a safe and non-toxic 3,4-dihydroxybenzaldehyde synthetic method
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Embodiment Construction
[0008] In this example, p-hydroxybenzaldehyde is firstly put into carbon tetrachloride and heated to dissolve, then the mixed solution of bromine and carbon tetrachloride is added dropwise at lower temperature, after several hours of reaction, the reaction solution is filtered, the solid is recrystallized, and after drying, 3- Bromo-4-hydroxybenzaldehyde, add the obtained 3-bromo-4-hydroxybenzaldehyde and catalyst into sodium hydroxide solution, put it in an autoclave and heat it to 150°C under a certain pressure, react for 1h, filter the reaction solution, and use Adjust the pH value to about 5 with hydrochloric acid aqueous solution, stir for 0.5 h, extract twice with ether, dry the organic phase and reflux to obtain the product.
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The invention discloses a synthetic method for 3,4-dihydroxybenzaldehyde. The method comprises the following steps: firstly, dissolving p-hydroxy benzaldehyde by using an organic solution, controllingthe temperature, slowly adding bromine dropwise, performing a reaction for a period of time, performing filtration, performing recrystallization, and performing drying to obtain 3-bromo-4-hydroxybenzaldehyde; and adding an alkali solution to dissolve the 3-bromo-4-hydroxybenzaldehyde and a catalyst, adding the obtained solution into an autoclave, performing heating to 150 DEG C, performing a reaction under stirring for 1 h, performing filtration, adjusting the pH value of the filtrate by using dilute hydrochloric acid, performing a reaction under stirring for 0.5 h, performing extraction twice by using an organic solution, combining the organic phases, performing drying by using saturated brine, and evaporating a solvent to obtain the 3,4-dihydroxybenzaldehyde. The raw materials are easyto obtain, and the method shortens the reaction route, increases the overall yield, is simple to operate and easy to implement, has low costs, and is suitable for industrial production.
Description
technical field [0001] The invention belongs to the field of compound synthesis, in particular to a synthesis method of 3,4-dihydroxybenzaldehyde. Background technique [0002] 3,4-Dihydroxybenzaldehyde is an important organic synthesis raw material and pharmaceutical intermediate, which can condense with compounds containing active hydrogen and ammonia. There are many traditional methods for synthesizing 3,4-dihydroxybenzaldehyde, but these methods have many synthetic steps and are relatively cumbersome, and the raw materials are all toxic. At present, the main source of 3,4-dihydroxybenzaldehyde in my country is from import. Contents of the invention [0003] The purpose of the present invention is to solve the problems of cumbersome steps and toxic raw materials in the existing traditional synthesis method, and provide a safe and non-toxic synthesis method of 3,4-dihydroxybenzaldehyde. [0004] The present invention is achieved through the following technical solutions...
Claims
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IPC IPC(8): C07C47/565C07C45/63C07C45/64
CPCC07C45/63C07C45/64C07C47/565
Inventor 王存亮许灵艳严学文黄焕军王小桥胡婷
Owner 胡婷
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