Method for synthesizing 4-methyl-5-(2- ethoxy) thiazole

A synthesis method and hydroxyethyl technology, applied in directions such as organic chemistry, can solve the problems of low product quality, complex process steps and high production costs, and achieve the effects of high product quality, simple process steps and low production costs

Inactive Publication Date: 2014-05-07
BENGBU COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In the reaction step of the synthesis method of 4-methyl-5-(2-hydroxyethyl)thiazole provided by the prior art, thiourea is used, so the extra amine group ...

Method used

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  • Method for synthesizing 4-methyl-5-(2- ethoxy) thiazole
  • Method for synthesizing 4-methyl-5-(2- ethoxy) thiazole
  • Method for synthesizing 4-methyl-5-(2- ethoxy) thiazole

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Embodiment 1

[0024] A synthetic method for 4-methyl-5-(2-hydroxyethyl)thiazole, comprising the following steps:

[0025] (1) Oxidation: Add 100 parts by mass of α-acetyl-γ-butyrolactone into a closed reaction kettle with a stirring and cooling device, slowly add 80 parts by mass of sulfonyl chloride dropwise under stirring, and keep the temperature at 40- Under the condition of 42℃, continue to stir for 1.5h, then use CaCl 2 After drying, filter to obtain α-acetyl-α-chloro-γ-butyrolactone;

[0026] (2) Hydrolytic decarboxylation: Take 100 parts by mass of α-acetyl-α-chloro-γ-butyrolactone prepared in step (1), add it to a closed reactor with a stirring and condensing reflux device, and then add 77 parts by mass Parts mass fraction is 5% dilute sulfuric acid or 160 mass parts mass fraction is 5% hydrochloric acid, heated to boiling reflux state, after reacting for 5h, the reaction solution was extracted 3 times with dichloromethane, and the amount of dichloromethane each time was 60 parts...

Embodiment 2

[0030] A synthetic method for 4-methyl-5-(2-hydroxyethyl)thiazole, comprising the following steps:

[0031] (1) Oxidation: Add 100 parts by mass of α-acetyl-γ-butyrolactone into a closed reaction kettle with a stirring and cooling device, slowly add 80 parts by mass of sulfonyl chloride dropwise under stirring, and keep the temperature at 40- Under the condition of 42℃, continue to stir for 2h, then use CaCl 2 After drying, filter to obtain α-acetyl-α-chloro-γ-butyrolactone;

[0032] (2) Hydrolytic decarboxylation: Take 100 parts by mass of α-acetyl-α-chloro-γ-butyrolactone prepared in step (1), add it to a closed reactor with a stirring and condensing reflux device, and then add 77 parts by mass Parts mass fraction is 5% dilute sulfuric acid or 160 mass parts mass fraction is 5% hydrochloric acid, heated to boiling reflux state, after reacting for 7h, the reaction solution was extracted 3 times with dichloromethane, each time dichloromethane consumption was 60 parts by mass...

Embodiment 3

[0036] A synthetic method for 4-methyl-5-(2-hydroxyethyl)thiazole, comprising the following steps:

[0037] (1) Oxidation: Add 100 parts by mass of α-acetyl-γ-butyrolactone into a closed reaction kettle with a stirring and cooling device, slowly add 80 parts by mass of sulfonyl chloride dropwise under stirring, and keep the temperature at 40- Under the condition of 42℃, continue to stir for 2.5h, then use CaCl 2 After drying, filter to obtain α-acetyl-α-chloro-γ-butyrolactone;

[0038] (2) Hydrolytic decarboxylation: Take 100 parts by mass of α-acetyl-α-chloro-γ-butyrolactone prepared in step (1), add it to a closed reactor with a stirring and condensing reflux device, and then add 77 parts by mass Parts mass fraction is 5% dilute sulfuric acid or 160 mass parts mass fraction is 5% hydrochloric acid, heated to boiling reflux state, after reacting for 6h, the reaction solution was extracted 3 times with dichloromethane, each time the amount of dichloromethane was 60 parts by ...

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Abstract

The invention provides a method for synthesizing 4-methyl-5-(2- ethoxy) thiazole. According to the method, the 4-methyl-5-(2- ethoxy) thiazole is prepared by using alpha-acetyl-gamma-butyrolactone through oxidation, hydrolyzed decarboxylation, synthesis and other steps. Thioformamide is utilized to replace thiourea in the method, so that the diazotizing and hydrolyzing steps for removing amidogen which is generated on a thiazole ring due to use of thiourea can be omitted, the process steps are simple, the product quality can be improved, and the production cost can be reduced.

Description

technical field [0001] The invention relates to a synthesis method of 4-methyl-5-(2-hydroxyethyl)thiazole. Background technique [0002] 4-Methyl-5-(2-hydroxyethyl)thiazole has a distinct nutty aroma and can be used for flavoring products such as dairy products and nuts. 4-Methyl-5-(2-hydroxyethyl)thiazole is also an important pharmaceutical intermediate. Its structural formula is: [0003] [0004] In the reaction step of the synthesis method of 4-methyl-5-(2-hydroxyethyl)thiazole provided by the prior art, thiourea is used, so the extra amine group generated on the thiazole ring must have diazo and hydrolysis steps, so that the process steps are complicated, the product quality is low, and the production cost is high. Contents of the invention [0005] The technical problem to be solved in the present invention is to provide a synthetic method of 4-methyl-5-(2-hydroxyethyl)thiazole, which can be used to prepare 4-methyl-5-(2- hydroxyethyl) thiazole, and the synthe...

Claims

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Application Information

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IPC IPC(8): C07D277/24
CPCC07D277/24
Inventor 郑桂富
Owner BENGBU COLLEGE
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