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Synthesis method of methyl o-anisate

A technology of methyl o-methoxybenzoate and salicylic acid, which is applied in the field of organic compound synthesis, can solve problems such as high power consumption, slow decomposition speed, restrict large-scale production, etc., and achieves reduction of reaction cycle, simplified processing difficulty, The effect of shortening the process flow

Inactive Publication Date: 2016-05-11
苏州诚和医药化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The disadvantage is that the dimethyl sulfate used produces a large amount of sodium monomethyl sulfate as a by-product. Because it is relatively stable, it can be decomposed into sodium sulfate under high temperature above 100°C under alkaline conditions, and the decomposition speed is extremely slow. Generally, it takes 8 to 12 hours to completely decompose the base, and the power consumption is extremely high, which seriously restricts its large-scale production.

Method used

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  • Synthesis method of methyl o-anisate
  • Synthesis method of methyl o-anisate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] like figure 2 In the synthetic route shown, 69g (0.50mol) of salicylic acid, 138ml of water, 70g (1.25mol) of potassium hydroxide will be added to the reaction flask equipped with an exhaust gas absorption device, and the stirring speed will be adjusted to 100 rpm. Cool the material to 10°C, start to feed methyl bromide slowly, control the speed of feeding methyl bromide to ensure that no methyl bromide gas overflows, and control the temperature not to exceed 20°C, stop feeding methyl bromide when the methyl bromide reaches 95g (1.0mol), let stand, take For the lower water layer sample, add hydrochloric acid to adjust the pH to 3~4, extract with ethyl acetate, spot the extract (developer ethyl acetate:petroleum ether=30:70), observe only one product spot (no raw materials and intermediate products) The reaction is over, otherwise, continue to feed 1.45g (0.015mol) of methyl bromide until the reaction is complete. In this test, add 3 times to complete the reaction. Sto...

Embodiment 2

[0021] like figure 2 In the synthetic route shown, 69g (0.50mol) of salicylic acid, 150ml of water, 56g (1.00mol) of potassium hydroxide will be added to the reaction flask equipped with an exhaust gas absorption device, and the stirring speed will be adjusted to 80 rpm. Cool the material to 15°C, start to feed methyl bromide slowly, control the speed of feeding methyl bromide to ensure that no methyl bromide gas overflows, and at the same time control the temperature not to exceed 20°C, when the methyl bromide reaches 95g (1.0mol), suspend the feeding of methyl bromide, stand still, take For the lower water layer sample, add hydrochloric acid to adjust the pH to 3~4, extract with ethyl acetate, spot the extract (developer ethyl acetate:petroleum ether=30:70), observe only one product spot (no raw materials and intermediate products) reaction. Stop stirring, let stand to separate the lower layer of waste water, waste water is concentrated under reduced pressure and evaporate...

Embodiment 3

[0024] like figure 2 In the synthetic route shown, 69g (0.50mol) of salicylic acid, 140ml of water, 59g (1.05mol) of potassium hydroxide will be added to the reaction flask equipped with an exhaust gas absorption device, and the stirring speed will be adjusted to 120 rpm. Cool the material to 13°C, start slowly feeding methyl bromide, control the speed of feeding methyl bromide to ensure that no methyl bromide gas overflows, and at the same time control the temperature not to exceed 20°C, stop feeding methyl bromide when the methyl bromide reaches 95g (1.0mol), let stand, take For the lower water layer sample, add hydrochloric acid to adjust the pH to 3~4, extract with ethyl acetate, spot the extract (developer ethyl acetate:petroleum ether=30:70), observe only one product spot (no raw materials and intermediate products) The reaction is over, otherwise, continue to supplement 2.375g (0.025mol) of methyl bromide until the reaction is complete. In this test, add 4 times to com...

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Abstract

The invention provides a synthesis method of methyl o-anisate. The method is as below: preparing salicylic acid and potassium hydroxide into an aqueous solution, adding the aqueous solution into a reactor, controlling the temperature at 10-20 DEG C, introducing methyl bromide under stirring, conducting board pointing to trace the extent of reaction; after the reaction, stopping stirring, allowing to stand at room temperature for stratification, separating waste water containing potassium bromide at the lower layer, and concentrating to obtain a by-product potassium bromide; washing the upper product by saturated brine, dying by anhydrous sodium sulfate, conducting vacuum distillation, and collecting fraction at 95-110 DEG C to obtain the methyl o-anisate. The synthesis method of methyl o-anisate has the advantages of shortened process, greatly reduced reaction period, reduction of the amount of three kings of wastes generated, simplified of difficulty in wastewater treatment, and great reduction of power consumption and equipment occupancy for treatment.

Description

technical field [0001] The invention belongs to the technical field of organic compound synthesis, in particular to a method for synthesizing methyl o-methoxybenzoate. Background technique [0002] The traditional synthetic method of methyl o-methoxybenzoate, such as figure 1 As shown, under alkaline conditions, salicylic acid reacts with dimethyl sulfate to generate o-methoxybenzoic acid, and then synthesizes methyl o-methoxybenzoate with methanol under sulfuric acid catalysis. The disadvantage is that the dimethyl sulfate used produces a large amount of sodium monomethyl sulfate as a by-product. Because it is relatively stable, it can be decomposed into sodium sulfate under high temperature above 100°C under alkaline conditions, and the decomposition speed is extremely slow. Generally, it takes 8 to 12 hours to completely decompose the base, and the power consumption is extremely high, which seriously restricts its large-scale production. The present invention adopts sal...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/11C07C69/92C01D3/10
CPCC07C67/11C01D3/10C07C69/92
Inventor 夏秋景
Owner 苏州诚和医药化学有限公司
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