Preparation process of duloxetine

A preparation process and technology of duloxetine, applied in the field of chemical drug preparation, can solve the problems of complexity, incomplete hydrolysis, influence on the purity of duloxetine, etc., and achieve high production safety, guaranteed purity and high reaction yield. Effect

Inactive Publication Date: 2017-09-29
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

However, the preparation operation of duloxetine in the prior art is relatively complicated, and the hydrolysis reaction used is ofte

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] The present invention proposes a preparation process of duloxetine, comprising the steps of:

[0021] S1: select thiophene, 2-acetylthiophene, 3-chloropropionyl chloride and 1-fluoronaphthalene as raw materials;

[0022] S2: Put thiophene and 2-acetylthiophene in the reactor, raise the temperature in the reactor to 70 degrees Celsius, mix them evenly and stir them, then add 3-chloropropionyl chloride, and Under the effect of reaction, generate 3-chloro-1-(2-thiophene)-acetone;

[0023] S3: Place the 3-chloro-1-(2-thiophene)-acetone in S2 in an environment of 60 degrees Celsius, and slowly add sodium borohydride to it, and mix and stir in real time during the addition, so as to obtain 3- Chloro-1-(2-thiophene)-propanol;

[0024] S4: After the above is completed, add the mixed solution to 3-chloro-1-(2-thiophene)-propanol again, and stir at 100 degrees Celsius for 10 minutes to generate a mixture A;

[0025] S5: Pass 1-fluoronaphthalene into the mixture A, lower the te...

Embodiment 2

[0033] The present invention proposes a preparation process of duloxetine, comprising the steps of:

[0034] S1: select thiophene, 2-acetylthiophene, 3-chloropropionyl chloride and 1-fluoronaphthalene as raw materials;

[0035] S2: Put thiophene and 2-acetylthiophene in the reactor, raise the temperature in the reactor to 75 degrees Celsius, mix them evenly and stir them, then add 3-chloropropionyl chloride, and Under the effect of reaction, generate 3-chloro-1-(2-thiophene)-acetone;

[0036] S3: Place the 3-chloro-1-(2-thiophene)-acetone in S2 in an environment of 70 degrees Celsius, and slowly add sodium borohydride to it, and mix and stir in real time during the addition, so as to obtain 3- Chloro-1-(2-thiophene)-propanol;

[0037] S4: After the above is completed, add the mixed solution to 3-chloro-1-(2-thiophene)-propanol again, and stir at 105 degrees Celsius for 13 minutes to generate a mixture A;

[0038] S5: Pass 1-fluoronaphthalene into the mixture A, lower the te...

Embodiment 3

[0046] The present invention proposes a preparation process of duloxetine, comprising the steps of:

[0047] S1: select thiophene, 2-acetylthiophene, 3-chloropropionyl chloride and 1-fluoronaphthalene as raw materials;

[0048] S2: Put thiophene and 2-acetylthiophene in the reactor, raise the temperature in the reactor to 80 degrees Celsius, mix them evenly and stir them, then add 3-chloropropionyl chloride, and Under the effect of reaction, generate 3-chloro-1-(2-thiophene)-acetone;

[0049] S3: Place the 3-chloro-1-(2-thiophene)-acetone in S2 at an environment of 80 degrees Celsius, and slowly add sodium borohydride to it, and mix and stir in real time during the addition, thereby obtaining 3- Chloro-1-(2-thiophene)-propanol;

[0050] S4: After the above is completed, add the mixed solution to 3-chloro-1-(2-thiophene)-propanol again, and stir at 110 degrees Celsius for 16 minutes to generate a mixture A;

[0051] S5: Pass 1-fluoronaphthalene into the mixture A, lower the ...

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PUM

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Abstract

The invention discloses a preparation process of duloxetine. The preparation process comprises the following steps: adding thiophene and 2-acetylthiophene into a reactor, heating until the temperature in the reactor is 70-90 DEG C, adding 3-chloropropionylchloride, reacting under the action of chiral acid so as to generate 3-chloro-1-(2-thiophene)-acetone, slowly adding sodium borohydride into 3-chloro-1-(2-thiophene)-acetone so as to obtain 3-chloro-1-(2-thiophene)-propanol, adding a mixed solution into 3-chloro-1-(2-thiophene)-propanol, introducing 1-fluoronaphthalene into a mixture A, cooling to 40-60 DEG C, stirring for 10-20 minutes for layering, adding strong base, washing, and drying by virtue of anhydrous sodium sulfate. The preparation process is simple in operation, high in reaction yield and production safety and suitable for large-scale industrial production, and the purity of the duloxetine can be guaranteed.

Description

technical field [0001] The invention relates to the technical field of chemical medicine preparation, in particular to a preparation process of duloxetine. Background technique [0002] With the rapid development of society, the pace of people's life and work is accelerating, and now people are under more and more pressure in life, leading to depression, world-weariness, loss, tension and depression. Therefore, the incidence of depression continues to rise, which seriously affects people. life. [0003] Therefore, the demand for duloxetine continues to increase, and duloxetine is mainly used clinically for the treatment of adult depression, moderate to severe stress urinary incontinence and diabetic peripheral neuralgia. In 2004, the U.S. FDA approved that its mechanism of action is the same as that of similar drug venlafaxine, but its inhibitory effect on norepinephrine reuptake is stronger than that of venlafaxine. The reuptake-consistent effect of epinephrine is more ba...

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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