A kind of preparation method of high-purity cis-3,5-dimethylpiperidine

A technology of dimethylpiperidine and lutidine, which is applied in the field of preparation of high-purity cis-3,5-dimethylpiperidine, can solve problems such as complex cis ratios, and achieve high commercial value and process Simple, great reference effect

Active Publication Date: 2019-06-07
VALIANT CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] It is relatively complicated to increase the cis ratio in the existing technology, so industrial production urgently needs to find a simple and suitable catalytic method and a simple and effective purification method to obtain high-purity cis-3,5-dimethylpiperidine

Method used

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  • A kind of preparation method of high-purity cis-3,5-dimethylpiperidine
  • A kind of preparation method of high-purity cis-3,5-dimethylpiperidine
  • A kind of preparation method of high-purity cis-3,5-dimethylpiperidine

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Experimental program
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Embodiment 1

[0039] Add 645.0g of 3,5-lutidine, 77.4g of neutral alumina, 12.9g of potassium carbonate, and 25.8g of ruthenium on carbon (5% effective content) into a 2L autoclave. Close the autoclave, replace with nitrogen 6 times, and replace with hydrogen 6 times. After charging and heating to a hydrogen pressure of 9.0MPa and 150°C, the hydrogen pressure will drop significantly during the reaction process. The heat preservation and pressure holding reaction lasted for 5.0 hours, and the complete reaction of 3,5-lutidine was detected. The reaction crude product was obtained by suction filtration. The rate is 96.8%. Gas chromatography analysis showed that the purity of cis-3,5-dimethylpiperidine was 84.5%, and the purity of trans-3,5-dimethylpiperidine was 15.2%.

[0040] The 2L three-necked bottle is equipped with a mechanical stirrer, a thermometer, and a drying tube. Add the above reaction crude product, 340.0g n-hexane, and 35.0g absolute ethanol into a 2L three-necked flask. Afte...

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Abstract

The invention relates to a preparation method of high-purity cis-3,5-dimethylpiperidine, belonging to the field of organic synthesis. Using 3,5-lutidine as a raw material, 3,5-dimethylpyridine is obtained through catalytic hydrogenation reaction. The crude methylpiperidine is purified by precipitation to obtain high-purity cis-3,5-dimethylpiperidine, and its cis gas chromatographic purity is more than 99.5%. In the present invention, by introducing neutral alumina and alkali, the combination mode of pyridine molecules and catalyst molecules in the hydrogenation process is changed, which is beneficial to the generation of cis-isomers, and can obtain crude products directly used in pharmaceutical production; 99.5% of the cis isomer, there is no such high-purity report in the synthesis and separation of 3,5-dimethylpiperidine cis, in the synthesis and purification of piperidine derivatives and industrial production applications, it has greater Reference significance and high commercial value.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a preparation method of high-purity cis-3,5-dimethylpiperidine. Background technique [0002] Cis-3,5-dimethylpiperidine is a derivative of piperidine, which is widely used in the preparation of antifungal agents and plant growth regulators. [0003] Cis-3,5-dimethylpiperidine is also used as an intermediate to prepare aminomethylheterocyclic insecticide compounds and compounds that can regulate eating behavior and related diseases, including obesity, Diabetes, cancer (tumours), inflammatory diseases, depression, stress-related diseases and Alzheimer's disease. In addition, cis-3,5-dimethylpiperidine is also very useful in the preparation of carbon-20-dihydro-dehydro-(cyclic amino) derivatives of macrolide antibiotics and in the preparation of molecular sieves. [0004] There are two existing methods for synthesizing 3,5-dimethylpiperidine: furanamine method and hyd...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D211/12
CPCC07B2200/09C07D211/12
Inventor 孙虎姜春晓付文岗孙晟源迟鹏利迟乃乔
Owner VALIANT CO LTD
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