Preparation method of methyl o-methoxybenzoate

A technology of methyl o-methoxybenzoate and methyl methoxybenzoate, which is applied in the field of organic compound synthesis, can solve problems such as high power consumption, restrictions on large-scale production, and slow decomposition speed, so as to reduce the reaction cycle, The effect of simplifying the difficulty of processing and shortening the process flow

Inactive Publication Date: 2016-04-06
苏州诚和医药化学有限公司
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Benefits of technology

This new compound can be made by reacting benzene sulfonamide (BSO) or other chemicals together at room temperature without generating harmful substances like ammonia gas that could cause environmental concerns during disposal processes. It also makes it easier for organic solvents used in cleanup operations to break down into small molecules which help remove unwanted materials from waterways more effectively.

Problems solved by technology

This patented technical problem addressed in this patents relates to improving methods for producing methionone (MU) from formaldehydes or other starting materials while minimizing excessive use of chemical resources during manufacturing processes.

Method used

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  • Preparation method of methyl o-methoxybenzoate
  • Preparation method of methyl o-methoxybenzoate

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Embodiment 1

[0017] Such as figure 2 In the synthetic route shown, 69g (0.50mol) of salicylic acid, 138ml of water, and 67g (1.2mol) of potassium hydroxide are added to the reaction flask equipped with an exhaust gas absorption device, and the stirring speed is 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. Stop s...

Embodiment 2

[0020] Such as 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 evapor...

Embodiment 3

[0023] Such as 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 ...

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Abstract

The invention provides a preparation method of methyl o-methoxybenzoate. The method comprises the following steps: preparing salicylic acid and potassium hydroxide in a molar ratio of 1:(2-2.4) into an aqueous solution and adding into a reaction device; controlling the temperature to 10-20 DEG C; introducing bromomethane in a stirring condition while performing point-plate tracking of the reaction degree; after the reaction is complete, stopping stirring and standing for layering at room temperature; separating out the potassium bromide-containing wastewater on the lower layer, and concentrating to obtain a byproduct potassium bromide; washing the upper-layer product with saturated salt solution; drying with anhydrous sodium sulfate and performing reduced-pressure distillation; and collecting the fraction at 95-110 DEG C to obtain methyl o-methoxybenzoate. According to the preparation method of methyl o-methoxybenzoate provided by the invention, the technological process is shortened, the reaction time is remarkably reduced, the generation of three wastes is reduced, the wastewater treatment difficulty is relieved, and the treatment power consumption and equipment occupation are greatly reduced.

Description

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Claims

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Application Information

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Owner 苏州诚和医药化学有限公司
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