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A kind of synthesis technique of n-methyl-5-hexen-1-amine

A synthesis process, hexene technology, applied in the preparation of amino-substituting functional groups, organic chemistry, etc., can solve the problems of safety hazards, low hydrogen explosion limit, etc., and achieve the effects of eliminating safety hazards, simple post-processing, and high product purity

Active Publication Date: 2020-07-24
上海仁实医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Sodium hydride is used as a reaction reagent in the above-mentioned process, and the by-product after the sodium hydride reaction is hydrogen, and the explosion limit of hydrogen is low and wide, which is a potential safety hazard in production. Therefore, a new technical solution needs to be proposed to solve the above technical problems

Method used

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  • A kind of synthesis technique of n-methyl-5-hexen-1-amine
  • A kind of synthesis technique of n-methyl-5-hexen-1-amine
  • A kind of synthesis technique of n-methyl-5-hexen-1-amine

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Embodiment 1

[0026] Embodiment 1: a kind of synthetic technique of N-methyl-5-hexen-1-amine, comprises the following steps: adding mass fraction in reaction bottle is the methylamine methanol solution of 25%, the content of methylamine is 2 equivalents , then add 1 equivalent of 6-bromo-1-hexene to the reaction flask, stir, heat the oil bath to 40°C, react for 3 hours, cool down to 20°C, add 0.1 equivalent of stabilizer, the stabilizer is p-formaldehyde Oxyphenol, add 1 equivalent of sodium hydroxide, recover excess methylamine methanol solution under negative pressure, heat to 50°C, and distill under reduced pressure to obtain a colorless liquid, which is N-methyl-5-hexene- 1-amine, the yield is 63%, and the purity is 95%; the synthesis process is carried out according to the following reaction formula:

[0027]

Embodiment 2

[0028] Embodiment 2: a kind of synthetic technique of N-methyl-5-hexene-1-amine, differs from embodiment 1, comprises the following steps: adding mass fraction in reaction bottle is the methylamine of 25% Methanol solution, the content of methylamine is 2 equivalents, then add 1 equivalent of 6-bromo-1-hexene to the reaction flask, stir, heat the oil bath to 45 °C, react for 2.5 hours, cool to 20 °C, add 0.1 Equivalent stabilizer, the stabilizer is p-methoxyphenol, add 1 equivalent of sodium hydroxide, recover excess methylamine methanol solution under negative pressure, heat to 55 ° C, and distill under reduced pressure to obtain a colorless liquid, which is N-methyl-5-hexen-1-amine, yield 64%, purity 95.2%.

Embodiment 3

[0029] Embodiment 3: a kind of synthetic technique of N-methyl-5-hexene-1-amine, differs from embodiment 1 in that, comprises the following steps: adding mass fraction in reaction bottle is the methylamine of 25% Methanol solution, the content of methylamine is 2 equivalents, then add 1 equivalent of 6-bromo-1-hexene to the reaction flask, stir, heat the oil bath to 50 ° C, react for 2 hours, cool down to 20 ° C, add 0.1 Equivalent stabilizer, the stabilizer is p-methoxyphenol, add 1 equivalent of sodium hydroxide, recover excess methylamine methanol solution under negative pressure, heat to 60°C, and distill under reduced pressure to obtain a colorless liquid, which is N-methyl-5-hexen-1-amine, yield 62%, purity 95.1%.

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Abstract

The invention discloses a synthesizing process of N-methyl-5-hexene-1-amine, and relates to the technical field of medicine synthesis and removes the potential safety hazard that explosive hydrogen isgenerated in the existing process. The synthesizing process comprises the following steps: adding methylamine solution containing methylamine and a solvent into a reaction flask and then adding 6-bromine-1-hexene into the reaction flask, wherein the molar equivalent of methylamine is greater than that of 6-bromine-1-hexene; stirring the mixture; performing oil-bath heating to 40-50 DEG C, performing a reaction for 2-3h, cooling to 20 DEG C, adding a stabilizing agent, then adding sodium hydroxide, recycling excessive methylamine solution under negative pressure, heating to 50-60 DEG C, and performing reduced pressure distillation, so as to obtain colorless liquid, namely, the N-methyl-5-hexene-1-amine. According to the process, the explosive hydrogen is not generated, the synthesizing process is safe, no organic solvent extraction process exists, the process is environmentally friendly, and the product purity is high.

Description

technical field [0001] The invention relates to the technical field of medicine synthesis, more specifically, it relates to a synthesis process of N-methyl-5-hexen-1-amine. Background technique [0002] N-methyl-5-hexen-1-amine is a widely used pharmaceutical and chemical intermediate, one end of which is a secondary amine, and the other end has an alkenyl group at the end of the alkyl group. These two groups can undergo various reactions with other active groups in chemical reactions, such as: alkylation reactions with alkyl halides, amide compounds with carboxylic acids, acid chlorides, and ester groups, and aldehydes and ketones The compound can generate Schiff base, and then reductive amination to generate tertiary amine; the double bond at the other end can be coupled, Michael addition, hydrogenation, or oxidized into alcohol group and aldehyde group; its self-generation can undergo hydrogenation and ring closure to generate pyrrole Alkylamines are important acid-bindi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C211/21C07C209/08
CPCC07C209/08C07C211/21
Inventor 宋东李文杰林长学
Owner 上海仁实医药科技有限公司
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