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Preparation process of sodium 3-methyl salicylate

A sodium methyl salicylate and preparation technology, which is applied in carboxylate preparation, organic chemistry, bulk chemical production, etc., can solve the problem that the number of patents is small, hindering the large-scale application of 3-methyl salicylate, etc. problem, to achieve the effect of mild and not harsh reaction conditions, large-scale large-scale production and application, and high product purity

Pending Publication Date: 2022-08-02
SUZHOU YACOO SCI CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At the same time, the number of patents about the preparation of 3-methylsalicylate sodium is relatively small, which cannot solve the problems in the above-mentioned preparation method, so the preparation process of 3-methylsalicylate sodium will hinder the production of 3-methylsalicylate. Large-scale application of sodium sylate in organic intermediates

Method used

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  • Preparation process of sodium 3-methyl salicylate
  • Preparation process of sodium 3-methyl salicylate
  • Preparation process of sodium 3-methyl salicylate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] A preparation process of sodium 3-methylsalicylate, comprising the following preparation steps:

[0056] (1) Preparation step 1:

[0057]

[0058] In the reactor, 1 mole of compound 1 was reacted with formaldehyde and hydrogen chloride; the substance ratio of compound 1, formaldehyde and hydrogen chloride was 1:1.1:1.1, the reaction solvent was DMF, the reaction temperature was 80°C, and the reaction pressure was 0.5 MPa, the reaction time is 4 hours, the reaction is completed, sodium hydroxide solution is added, and the reaction is continued for 4 hours. After the reaction is completed, it is lowered to room temperature, the organic phase is collected, and spin-dried to obtain compound 2.

[0059] (2) preparation step 2:

[0060]

[0061] In the reactor, 1 mole of compound 2 in the above formula was reacted with hydrogen peroxide; the substance ratio of compound 2 to hydrogen peroxide was 1:1.5; the solvent was THF, the reaction temperature was 50°C, and the rea...

Embodiment 2

[0069] A preparation process of sodium 3-methylsalicylate, comprising the following preparation steps:

[0070] (1) Preparation step 1:

[0071]

[0072] In a reactor, combine 1 mole of compound 1 with formaldehyde and Br 2 Reaction; compound 1, formaldehyde, Br 2 The amount ratio of the substances is 1:1.1:1.5, the reaction solvent is THF, the reaction temperature is 60 ° C, the reaction pressure is normal pressure, the reaction time is 6 hours, the reaction is completed, the sodium hydroxide solution is added, and the reaction is continued for 2 hours. After completion, it was lowered to room temperature, the organic phase was collected, and spun dry to obtain compound 2.

[0073] (2) preparation step 2:

[0074]

[0075] In the reactor, 1 mole of compound 2 in the above formula was reacted with potassium permanganate; the substance ratio of compound 2 to potassium permanganate was 1:1.2; the solvent was acetonitrile, the reaction temperature was 30°C, and the react...

Embodiment 3

[0083] A preparation process of sodium 3-methylsalicylate, comprising the following preparation steps:

[0084] (1) Preparation step 1:

[0085]

[0086] In the reactor, 1 mole of compound 1 was reacted with formaldehyde and thionyl chloride; the substance ratio of compound 1, formaldehyde and thionyl chloride was 1:1.5:2, the solvent was DMSO, and the reaction temperature was 60°C , the reaction pressure is normal pressure, and the reaction time is 6 hours. After the reaction is completed, sodium hydroxide solution is added, and the reaction is continued for 2 hours.

[0087] (2) preparation step 2:

[0088]

[0089] In the reactor, 1 mole of compound 2 in the above formula was reacted with ammonium persulfate; the substance ratio of compound 2 to sulfuric acid was 1:1.2; the solvent was acetone, the reaction temperature was 60°C, and the reaction pressure was normal pressure, The reaction time was 3 hours, the reaction was completed, the reaction was continued to com...

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Abstract

The invention discloses a preparation process of sodium 3-methyl salicylate, which comprises the following steps: reacting a compound 1 with a reagent A, and performing at least one of hydrolysis reaction and esterification reaction to obtain a compound 2; performing oxidation reaction on the compound 2 to prepare a compound 3; the compound 3 is subjected to at least one of hydrolysis reaction and acid-alkali treatment to prepare 3-methyl sodium salicylate; according to the preparation process, a high-purity product is obtained through initial raw material optimization, preparation and purification processes, and the obtained sodium 3-methyl salicylate meets the requirements of purity, impurity content, cost and the like of an intermediate; moreover, the preparation process is relatively simple to operate, mild and not harsh in reaction condition, free of high-pressure and high-temperature reactions and the like, easily available in raw materials, short in reaction production period, high in yield and beneficial to reduction of product cost, and large-batch and large-scale production can be realized.

Description

technical field [0001] The invention belongs to the technical field of organic intermediates, and in particular relates to a preparation process of sodium 3-methylsalicylate. Background technique [0002] Sodium 3-methylsalicylic acid, English name 3-methylsalicylic acid sodium salt, CAS number 32768-20-0, is an important organic intermediate. [0003] Existing technologies such as Kh.A.Suerbaev, etc. are based on CO 2 To prepare methyl salicylic acid and its sodium salt by reacting carbon source and alkyl phenol, but the preparation method CO 2 It is often necessary to form sodium ethyl carbonate with sodium ethoxide at a high pressure of 10 atm and a high temperature of over 180 °C, and then react with o-cresol to obtain 3-methylsalicylic acid, and further obtain its sodium salt. This method not only needs to carry out the reaction under high temperature and high pressure, but the yield of the prepared 3-methylsalicylic acid is only 38%, and the yield is low. [0004] A...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/41C07C65/10
CPCC07C51/412C07C51/265C07C37/00C07C37/11C07C65/10C07C39/11C07C39/24Y02P20/55
Inventor 袁永坤蒋玉贵夏金成
Owner SUZHOU YACOO SCI CO LTD
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