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Duloxetine preparation method

A technology of duloxetine and thiophene, which is applied in the field of duloxetine preparation, can solve the problems of difficult preparation, high cost, unfavorable production, etc., and achieve the effects of fast reaction speed, easy preparation and low cost

Inactive Publication Date: 2017-08-08
武汉励合生物医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the preparation method of duloxetine in the prior art, its raw materials are often difficult to prepare, or the cost is too high, which is not conducive to large-scale production, thereby increasing the cost of the drug

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] The present invention proposes a kind of preparation method of duloxetine, comprises the steps:

[0021] S1: select thiophene and 2-chloroacetyl chloride as raw materials, and store in a sealed manner at 20°C for later use;

[0022] S2: Heat 2-chloroacetyl chloride into the reaction vessel to 60°C, add thiophene, shake gently, continue heating and stirring for 10 minutes, and obtain 2-chloroacetylthiophene through Friedel-Crafts acylation;

[0023] The preparation method of 2-chloroacetyl chloride comprises the following steps:

[0024] A1: Select trichlorethylene as a raw material and put it into a reaction vessel, add azobisisobutyronitrile as a catalyst, and heat to 95°C;

[0025] A2: Introduce oxygen into the above reaction vessel, continue the reaction under the pressure of 0.6MPa, keep the temperature of the oil bath at 105°C, and continue the reaction for 8 hours;

[0026] A3: Place the above reaction product under normal pressure and separate to obtain dichlor...

Embodiment 2

[0032] The present invention proposes a kind of preparation method of duloxetine, comprises the steps:

[0033] S1: select thiophene and 2-chloroacetyl chloride as raw materials, and store in a sealed manner at 21°C for later use;

[0034] S2: Heat 2-chloroacetyl chloride into the reaction vessel to 61°C, add thiophene, shake gently, continue heating and stirring for 10 minutes, and obtain 2-chloroacetylthiophene through Friedel-Crafts acylation;

[0035] The preparation method of 2-chloroacetyl chloride comprises the following steps:

[0036] A1: Select trichlorethylene as a raw material and put it into a reaction vessel, add azobisisobutyronitrile as a catalyst, and heat to 95°C;

[0037] A2: Introduce oxygen into the above reaction vessel, continue the reaction under the pressure of 0.6MPa, keep the temperature of the oil bath at 105°C, and continue the reaction for 8 hours;

[0038] A3: Place the above reaction product under normal pressure and separate to obtain dichlor...

Embodiment 3

[0044] The present invention proposes a kind of preparation method of duloxetine, comprises the steps:

[0045] S1: Select thiophene and 2-chloroacetyl chloride as raw materials, and store them in a sealed container at 22°C for later use;

[0046] S2: Heat 2-chloroacetyl chloride into the reaction vessel to 62°C, add thiophene, shake gently, continue heating and stirring for 10 minutes, and obtain 2-chloroacetylthiophene through Friedel-Crafts acylation;

[0047] The preparation method of 2-chloroacetyl chloride comprises the following steps:

[0048] A1: Select trichlorethylene as a raw material and put it into a reaction vessel, add azobisisobutyronitrile as a catalyst, and heat to 95°C;

[0049] A2: Introduce oxygen into the above reaction vessel, continue the reaction under the pressure of 0.6MPa, keep the temperature of the oil bath at 105°C, and continue the reaction for 8 hours;

[0050] A3: Place the above reaction product under normal pressure and separate to obtain...

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Abstract

The invention relates to the technical field of chemical synthesis, particularly to a duloxetine preparation method. The duloxetine preparation method comprises the following steps: choosing thiophene and 2-chloroacetyl chloride as raw materials, sealing and storing at 20-25 DEGC for standby application, putting 2-chloroacetyl chloride into a reaction vessel, heating to 60-65 DEGC, adding thiophene, slightly shaking evenly, continuing to heat, stirring for 10 minutes, obtaining 2-chloracetyl-thiophene through a friedel-crafts reaction, heating the produced 2-chloracetyl-thiophene to 80-100 DEGC, adding sodium cyanide into the reaction vessel, continuing to stir, heating for 10 minutes, conducting a cyano substitution reaction, and obtaining 3-hydroxy-3-(2-thiophene)-propionitrile. The cheap thiophene and 2-chloroacetyl chloride are chosen as the raw materials, the preparation is easy, the cost is low, the preparation is conducted through the conventional reactions, and the method has the advantages of low cost, easy preparation and high reaction speed.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a preparation method of duloxetine. Background technique [0002] Duloxetine is a selective serotonin (5-HT) and norepinephrine (NE) reuptake inhibitor. Preclinical studies have shown that duloxetine is a strong inhibitor of neuronal 5-HT and NE reuptake, and its inhibitory effect on dopamine reuptake is relatively weak. In vitro studies have shown that duloxetine has no significant affinity with dopaminergic receptors, adrenergic receptors, cholinergic receptors, histaminergic receptors, opioid receptors, glutamate receptors, and GABA receptors. Duloxetine does not inhibit monoamine oxidase. [0003] In the preparation method of duloxetine in the prior art, its raw materials are often difficult to prepare, or the cost is too high, which is not conducive to mass production, thereby increasing the cost of the drug. Contents of the invention [0004] The present inv...

Claims

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Application Information

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IPC IPC(8): C07D333/20
CPCC07D333/20
Inventor 彭凡李娜陈金利何峰叶志伟
Owner 武汉励合生物医药科技有限公司
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