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Salicylaldehyde synthesis method

A technology for the synthesis of o-hydroxybenzaldehyde, which is applied to the preparation of carbon-based compounds, chemical instruments and methods, and the preparation of carbonyl compounds by hydrolysis. Easy control, high product purity and yield, and short process flow

Inactive Publication Date: 2016-05-04
陈士忠
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The traditional production of o-hydroxybenzaldehyde is the ortho-formylation method of phenol. This method requires the use of the toxic solvent HMPA. The process is relatively long and has certain hazards to the human body. At the same time, the process control is difficult and there are many by-products. The purity of the final product is difficult to guarantee

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Embodiment 1, a kind of synthetic method of o-hydroxybenzaldehyde, used raw material is chloroform, phenol, sodium hydroxide, and this method forms through reflux, acidification, extraction, distillation, acidolysis, evaporation; 1000 milliliters mass concentration Add 40-50% sodium hydroxide solution into the reactor with condensing reflux device, put 150-250 grams of phenol, keep stirring, and heat in water bath to 55-65 ° C, add 300-350 grams of chloroform , raise the temperature to 70-80°C, and keep warm and reflux for 1-3 hours; acidification is to adjust the pH value of the reaction material to 2-3 with sulfuric acid with a mass concentration of 10-20%; distillation is to add the material to Ethyl acetate, stirring continuously for 15-25 minutes, heating to 60-65°C, the evaporated gas is recovered by condensation, when no condensate is formed, the temperature is raised to 75-80°C, the evaporated gas is recovered by condensation , when no condensate is formed, rais...

Embodiment 2

[0014] Embodiment 2, in the synthetic method of a kind of o-hydroxybenzaldehyde described in embodiment 1: the sodium hydroxide solution of 1000 milliliters 45% is joined in the reactor with condensation reflux device, puts into 200 grams of phenol, constantly Stir and heat to 60° C. in a water bath, add 320 g of chloroform, raise the temperature to 75° C., and keep at reflux for 2 hours.

Embodiment 3

[0015] Embodiment 3, in the synthetic method of a kind of o-hydroxybenzaldehyde described in embodiment 1: acidification is to adjust reactant pH value to 2-3 with 15% sulfuric acid of reaction mass.

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Abstract

The present invention relates to a salicylaldehyde synthesis method, wherein the used raw materials comprise chloroform, phenol, and sodium hydroxide, and the method comprises reflux, acidification, extraction, distillation, acidolysis and evaporation. The method concretely comprises: adding a sodium hydroxide solution, phenol and chloroform to a reactor, heating to a temperature of 70-80 DEG C, carrying out a reflux reaction for 2 h, adjusting the PH value of the reactant to 2-3 with sulfuric acid, standing the reaction material, separating to obtain an oil component, adding ethyl acetate, sequentially heating to temperatures of 60-65 DEG C, 75-80 DEG C and 175-185 DEG C, separately recovering the condensates and separating to obtain oil components, mixing the oil components and a sodium bisulfite solution, mixing the precipitate and sulfuric acid, separating to obtain an oil layer, evaporating the oil layer, and collecting the condensate. According to the present invention, the method has characteristics of short process, easy reaction process control, less by-product, high product purity, and high product yield.

Description

technical field [0001] The invention relates to a preparation technology of chemical raw materials, in particular to a synthesis method of o-hydroxybenzaldehyde. Background technique [0002] O-Hydroxybenzaldehyde is a fine chemical product with a wide range of uses, and is widely used in the synthesis of pesticides, medicines, spices, chelating agents, dye intermediates, etc. In terms of pesticides, halogenated salicylaldehyde, salicylaldehyde hydrazone and phenylhydrazone are all important raw materials for the preparation of herbicides, insecticides, fungicides and preservatives; in medicine, salicylaldehyde can be used to prepare antibacterial drugs, and as Production of intermediates of racemic pituitary-stimulating gonadal hormones and production of adrenaline-mimetic drugs and anti-cough and asthma drugs; also used in the preparation of porous plastics and as antioxidants for plastics, metal passivators for oil refining industries, etc. ; Low concentration of o-hydro...

Claims

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Application Information

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IPC IPC(8): C07C47/565C07C45/43C07C45/00
Inventor 陈士忠
Owner 陈士忠
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