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Production method of thiophene-2-ethylamine

A production method, thiophene technology, applied in the production field of thiophene-2-ethylamine, can solve the problems of product purity, low conversion rate, production efficiency, complicated process, etc., and achieve high product conversion rate and production efficiency, and simple process effect

Inactive Publication Date: 2021-02-09
菏泽鸿特药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, the existing production method of thiophene-2-ethylamine has problems such as complex process, low product purity, conversion rate and production efficiency, and therefore needs to be improved urgently.

Method used

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  • Production method of thiophene-2-ethylamine

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Effect test

Embodiment 1

[0024] This embodiment provides a kind of production method of thiophene-2-ethylamine, it comprises the following steps:

[0025] S1, put 2048kg thiophene-2-ethanol and 2000kg oxidant in 70m 3 Oxidation reaction in n-hexane gives thiophene-2-acetaldehyde.

[0026] S2. After reacting 1764kg of thiophene-2-acetaldehyde and 1500kg of hydroxylamine hydrochloride in 4000kg of 90% ethanol solution, extract with dichloromethane, dry over anhydrous magnesium sulfate, and distill to obtain thiophene-2- Acetaldehyde oxime.

[0027] S3, place 1884kg of thiophene-2-aldoxime and 1500kg of sodium borohydride in 6000kg of cold tetrahydrofuran solution for reduction reaction, then extract with ethyl acetate, dry over anhydrous magnesium sulfate, and distill under reduced pressure The product thiophene-2-ethylamine was obtained.

Embodiment 2

[0029] This embodiment provides a kind of production method of thiophene-2-ethylamine, it comprises the following steps:

[0030] S1, put 2048kg thiophene-2-ethanol and 2300kg oxidant in 90m 3 Oxidation reaction in n-hexane gives thiophene-2-acetaldehyde.

[0031] S2. After reacting 1764kg of thiophene-2-acetaldehyde and 1700kg of hydroxylamine hydrochloride in 7000kg of 95% ethanol solution, extract with dichloromethane, dry over anhydrous magnesium sulfate, and obtain thiophene-2- Acetaldehyde oxime.

[0032] S3, place 1884kg of thiophene-2-aldoxime and 1700kg of sodium borohydride in 8000kg of cold tetrahydrofuran solution for reduction reaction, then extract with ethyl acetate, dry over anhydrous magnesium sulfate, and distill under reduced pressure The product thiophene-2-ethylamine was obtained.

Embodiment 3

[0034] This embodiment provides a kind of production method of thiophene-2-ethylamine, it comprises the following steps:

[0035] S1, put 2048kg thiophene-2-ethanol and 2300kg oxidant in 75m 3 Oxidation reaction in n-hexane gives thiophene-2-acetaldehyde.

[0036] S2. After reacting 1764kg of thiophene-2-acetaldehyde and 1600kg of hydroxylamine hydrochloride in 5000kg of 92% ethanol solution, they were extracted with dichloromethane, dried over anhydrous magnesium sulfate, and distilled to obtain thiophene-2- Aldoxime.

[0037] S3, place 1884kg of thiophene-2-glyoxaldoxime and 1600kg of sodium borohydride in 6500kg of cold tetrahydrofuran solution for reduction reaction, then extract with ethyl acetate, dry over anhydrous magnesium sulfate, and distill under reduced pressure The product thiophene-2-ethylamine was obtained.

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Abstract

The invention is suitable for the technical field of chemical industry production, and provides a production method of thiophene-2-ethylamine. The production method comprises the steps of placing thiophene-2-ethanol and an oxidizing agent in a first solvent to carry out an oxidation reaction to obtain thiophene-2-acetaldehyde; putting thiophene-2-acetaldehyde and hydroxylamine hydrochloride into asecond solvent to react, and purifying to obtain thiophene-2-acetaldoxime; and putting thiophene-2-acetaldoxime and sodium borohydride into a third solvent to carry out reduction reaction, and purifying to obtain thiophene-2-ethylamine. The production method of thiophene-2-ethylamine provided by the invention is simple in process, and comprises the steps of by taking thiophene-2-ethanol as a rawmaterial, firstly preparing thiophene-2-acetaldehyde by an oxidation method, then preparing thiophene-2-acetaldoxime from thiophene-2-acetaldehyde and hydroxylamine hydrochloride, and then reducing thiophene-2-acetaldoxime into a product thiophene-2-ethylamine. The method has the advantages of high product purity, high product conversion rate and high production efficiency.

Description

technical field [0001] The invention belongs to the technical field of chemical production, and in particular relates to a production method of thiophene-2-ethylamine. Background technique [0002] Thiophene-2-ethylamine, namely 2-thienylethylamine, CAS registration number is 30433-91-1, chemical formula is C 6 h 9 NS. Thiophene-2-ethylamine is commonly used as a pharmaceutical intermediate, specifically as an antithrombotic drug clopidogrel intermediate. [0003] However, the existing production method of thiophene-2-ethylamine has problems such as complex process, low product purity, conversion rate and production efficiency, and therefore needs to be improved urgently. Contents of the invention [0004] The purpose of the embodiments of the present invention is to provide a production method of thiophene-2-ethylamine, aiming to solve the problems raised in the background technology. [0005] The embodiment of the present invention is achieved in this way, a producti...

Claims

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Application Information

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IPC IPC(8): C07D333/20
CPCC07D333/20
Inventor 殷文
Owner 菏泽鸿特药业有限公司
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