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Synthesis method of m-methoxybenzyl alcohol

A technology of m-methoxybenzyl alcohol and methoxybenzyl alcohol is applied in the synthesis field of m-methoxybenzyl alcohol, and can solve the problem of unsafe synthesis process of m-methoxybenzyl alcohol, low product yield and complicated process and other problems, to achieve the effect of high product yield, cheap and easy-to-obtain raw materials, and simple synthesis process

Active Publication Date: 2021-06-25
SINOPHARM CHEM REAGENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In view of the above-mentioned problems that the synthesis process of m-methoxybenzyl alcohol is unsafe, the product yield is not high and the process is complicated, the object of the present invention is to provide a m-methoxybenzyl alcohol with safe synthesis process, simple process and high product yield. The synthetic method of benzyl alcohol

Method used

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  • Synthesis method of m-methoxybenzyl alcohol

Examples

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Comparison scheme
Effect test

Embodiment 1

[0028] A kind of synthetic method of m-methoxybenzyl alcohol, comprises the steps:

[0029] One, the preparation of m-chlorobenzaldehyde condensed with ethylene glycol:

[0030] (1) Add m-chlorobenzaldehyde and toluene (solvent) in the reaction vessel, then add ethylene glycol and sulfuric acid and stir evenly, then heat to 100°C for condensation reaction for 7 hours, remove the toluene and ethylene glycol after the reaction , then rectifying, promptly obtains said ethylene glycol acetal m-chlorobenzaldehyde; The mol ratio between said m-chlorobenzaldehyde, ethylene glycol and said sulfuric acid in this step is 1:2:0.3;

[0031] Two, the preparation of ethylene glycol condensed m-methoxybenzaldehyde:

[0032] (1) Get 1mol of the gained ethylene glycol condensed m-chlorobenzaldehyde and dissolve it in the anhydrous methanol of 500mL and stir evenly to obtain a mixed solution;

[0033] (2) Under stirring conditions, add 1.2mol of sodium methoxide (condensing agent) to the mixe...

Embodiment 2

[0043] A kind of synthetic method of m-methoxybenzyl alcohol, comprises the steps:

[0044] One, the preparation of m-chlorobenzaldehyde condensed with ethylene glycol:

[0045] (1) Add m-chlorobenzaldehyde and xylene (solvent) in the reaction vessel, then add ethylene glycol and sulfuric acid and stir evenly, then heat to 120°C for condensation reaction for 5 hours, remove the toluene and ethylene glycol after the reaction Alcohol, rectifying then, promptly obtains described ethylene glycol acetal m-chlorobenzaldehyde; The mol ratio between described m-chlorobenzaldehyde, ethylene glycol and described sulfuric acid in this step is 1:3:0.1;

[0046] Two, the preparation of ethylene glycol condensed m-methoxybenzaldehyde:

[0047] (1) Get 0.5mol of the gained ethylene glycol condensed m-chlorobenzaldehyde and dissolve it in 500mL of anhydrous methanol and stir to obtain a mixed solution;

[0048] (2) Under stirring conditions, add 0.75mol of sodium methoxide (condensing agent...

Embodiment 3

[0056] A kind of synthetic method of m-methoxybenzyl alcohol, comprises the steps:

[0057] One, the preparation of m-chlorobenzaldehyde condensed with ethylene glycol:

[0058] (1) Add m-chlorobenzaldehyde and toluene (solvent) in the reaction vessel, then add ethylene glycol and sulfuric acid and stir evenly, then heat to 110°C for condensation reaction for 10 hours, remove the toluene and ethylene glycol after the reaction , then rectifying, promptly obtains said ethylene glycol acetal m-chlorobenzaldehyde; The mol ratio between said m-chlorobenzaldehyde, ethylene glycol and said sulfuric acid in this step is 1:5:0.5;

[0059] Two, the preparation of ethylene glycol condensed m-methoxybenzaldehyde:

[0060] (1) Get 0.8mol of gained ethylene glycol acetal m-chlorobenzaldehyde and be dissolved in the anhydrous methanol of 500mL and stir, obtain mixed solution;

[0061] (2) Under stirring conditions, add 0.8mol of sodium methoxide (condensing agent) to the mixed solution, he...

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Abstract

The invention discloses a synthesis method of m-methoxybenzyl alcohol. The synthesis method comprises the steps: (1) by taking ethylene glycol and m-chlorobenzaldehyde as raw materials and sulfuric acid as a catalyst, carrying out condensation reaction in a solvent to prepare ethylene glycol condensed m-chlorobenzaldehyde; (3) dissolving the ethylene glycol condensed m-chlorobenzaldehyde in an organic solvent to obtain a mixed solution; (4) adding a condensing agent into the mixed solution under a stirring condition, and heating for reaction to form a reaction system containing ethylene glycol condensed m-methoxybenzaldehyde; (5) evaporating to remove the organic solvent in the reaction system, then cooling, adjusting the pH value of the system, and carrying out phase splitting on the reaction system after the pH value is adjusted to obtain an organic phase I; (6) adding a catalyst and a metal reducing agent into the organic phase I, resolving acetal and reducing to obtain a reaction solution containing a crude product of m-methoxybenzyl alcohol; and (7) continuing to split phases of the reaction liquid to obtain an organic phase II, and washing, drying and rectifying the organic phase II to obtain refined m-methoxybenzyl alcohol.

Description

technical field [0001] The invention relates to the technical field of synthesis of pharmaceutical intermediates, in particular to a synthesis method of m-methoxybenzyl alcohol. Background technique [0002] 3-methoxybenzyl chloride, also known as m-methoxybenzyl chloride, is a key intermediate for the synthesis of new anti-cardiovascular drugs clonidine hydrochloride. M-methoxybenzyl alcohol (m-methoxybenzyl alcohol) is again the key intermediate for the synthesis of 3-methoxybenzyl chloride, so the synthesis of m-methoxybenzyl alcohol is very important. The method for producing 3-methoxybenzyl chloride mainly contains two kinds of methods using 3-methoxybenzaldehyde as raw material and 3-hydroxybenzaldehyde as raw material at present: (1) using 3-methoxybenzaldehyde The method of formaldehyde as raw material is: 3-methoxybenzaldehyde is hydrogenated and reduced by Raney nickel to obtain 3-methoxybenzyl alcohol, which is then obtained by halogenation with thionyl chloride;...

Claims

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Application Information

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IPC IPC(8): C07C41/26C07C43/23
CPCC07C41/26C07D317/22C07D317/16C07C43/23Y02P20/584
Inventor 郭建国吴孝兰夏晓晗孙蔚晨
Owner SINOPHARM CHEM REAGENT
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