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Preparation method of trans-3,5-dimethylpiperidine

A technology of dimethylpiperidine and lutidine, which is applied in the field of preparation of trans-3,5-dimethylpiperidine, can solve the problem of low proportion

Pending Publication Date: 2021-09-10
ANHUI XINGYU CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] Aiming at the low proportion of trans 3,5-dimethylpiperidine in the existing preparation of 3,5-dimethylpiperidine, the present invention provides a preparation of trans 3,5-dimethylpiperidine method, increasing the content ratio of trans-3,5-dimethylpiperidine

Method used

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  • Preparation method of trans-3,5-dimethylpiperidine

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Comparison scheme
Effect test

Embodiment 1

[0029] The preparation method of the trans 3,5-dimethylpiperidine of the present embodiment comprises the following steps:

[0030] A. Under hydrogen protection conditions, add 100g3,5-lutidine, 40g deionized water, 5g composite catalyst (the mass ratio of ruthenium carbon, nickel powder and metal iron acetate is 1:0.05:0.05) to the high pressure reaction React in the still, the reaction pressure of carrying out reaction is 30kg / cm 2 , the reaction temperature is 140°C, the reaction time is 5h, and after the reaction is completed, the crude product of 3,5-dimethylpiperidine is obtained by suction filtration;

[0031] B. Cool the crude 3,5-dimethylpiperidine obtained in step A to room temperature, take out the reaction mixture, and take the supernatant after standing still to obtain 3,5-dimethylpiperidine.

[0032] Since the product 3,5-dimethylpiperidine and the raw material 3,5-lutidine have a low boiling point, a relatively simple and fast gas chromatography method is adopt...

Embodiment 2

[0053] The preparation method of the trans 3,5-dimethylpiperidine of the present embodiment comprises the following steps:

[0054] A. Under hydrogen protection conditions, add 100g3,5-lutidine, 60g deionized water, 8g composite catalyst (the mass ratio of ruthenium carbon, nickel powder and metal zinc acetate is 1:0.08:0.08) to the high pressure reaction React in the still, the reaction pressure of carrying out reaction is 40kg / cm 2 , the reaction temperature is 150°C, the reaction time is 8h, and after the reaction is completed, the crude product of 3,5-dimethylpiperidine is obtained by suction filtration;

[0055] B. Cool the crude 3,5-dimethylpiperidine obtained in step A to room temperature, take out the reaction mixture, and take the supernatant after standing still to obtain 3,5-dimethylpiperidine.

[0056] The content of the trans isomer of the 3,5-dimethylpiperidine mixture detected by gas chromatography (GC) was 34.9%.

Embodiment 3

[0058] The preparation method of the trans 3,5-dimethylpiperidine of the present embodiment comprises the following steps:

[0059] A. Under hydrogen protection conditions, add 100g3,5-lutidine, 50g deionized water, 6g composite catalyst (the mass ratio of ruthenium carbon, nickel powder and metal magnesium acetate is 1:0.1:0.05) to the high pressure reaction React in the still, the reaction pressure of carrying out reaction is 35kg / cm 2 , the reaction temperature is 160°C, the reaction time is 6h, and after the reaction is completed, the crude product of 3,5-dimethylpiperidine is obtained by suction filtration;

[0060] B. Cool the crude 3,5-dimethylpiperidine obtained in step A to room temperature, take out the reaction mixture, and take the supernatant after standing still to obtain 3,5-dimethylpiperidine.

[0061] The content of the trans isomer of the 3,5-dimethylpiperidine mixture detected by gas chromatography (GC) was 32.7%.

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Abstract

The invention discloses a preparation method of trans-3,5-dimethylpiperidine, belonging to the technical field of chemical products. The method comprises the following steps: A, adding 3,5-dimethylpyridine, deionized water and a composite catalyst into a high-pressure reaction kettle for a reaction under the protection of hydrogen, and carrying out suction filtration after the reaction is finished to obtain a crude 3,5-dimethylpiperidine product; and B, cooling the crude 3,5-dimethylpiperidine product obtained in the step A to room temperature, taking out a reaction mixture, conducting standing, and taking supernatant liquid to obtain the trans-3,5-dimethylpiperidine. According to the invention, reaction conditions are mild and easy to control, reaction effect is good, and a trans content can reach 20-35%.

Description

technical field [0001] The invention belongs to the technical field of chemical products, and more specifically relates to a preparation method of trans-3,5-dimethylpiperidine. Background technique [0002] 3,5-Dimethylpiperidine is the main intermediate of the generic drug Tilmicosin, which is a special antibiotic for livestock and poultry animals and is used in a large amount; it is also the main component of environmentally friendly new material automobile exhaust adsorbent intermediate. 3,5-Dimethylpiperidine has two isomers, cis and trans, and the main method of synthesis is the tank-type hydrogenation process, using a hydrogenation catalyst to hydrogenate 3,5-lutidine to prepare 3,5-Dimethylpiperidine. In addition, there is furan amine method, wherein the production cost of furan amine method is relatively high, so industrial production generally adopts hydrogenation method for preparation. [0003] In order to solve the above problems, after retrieval, such as pate...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D211/12
CPCC07D211/12C07B2200/09
Inventor 张升张宽宇万红根刘进水张太亮
Owner ANHUI XINGYU CHEM
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