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Preparation method of methylamine

A technology for methyl amine and amine methylation, applied in the field of preparing methyl amine, can solve the problems of complex methyl amine production links, unstable organic catalysts, harsh reaction conditions, etc., to simplify the post-processing process and avoid device performance. Reduced, silicophilic effect

Active Publication Date: 2020-12-01
NANJING XIAOZHUANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Aiming at the technical problems existing in the prior art, the present invention provides a kind of preparation method of methylamine, to overcome the catalytic CO in the prior art 2 The metal catalysts for the preparation of methylamine are expensive, highly toxic, unstable organic catalysts, and harsh reaction conditions, resulting in complex production of methylamine and high manufacturing costs.

Method used

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  • Preparation method of methylamine
  • Preparation method of methylamine
  • Preparation method of methylamine

Examples

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Embodiment 1

[0041] This embodiment provides a method for preparing methylamine, wherein the catalyst used is dodecyldimethylamine caprolactone, the methylamine is 2-(methyl(phenyl)amino)ethanol, and methyl The reaction scheme of the amine is as follows:

[0042]

[0043] The preparation method of 2-(methyl (phenyl) amino) ethanol comprises the following steps:

[0044] Take a strictly dry Shrek reaction tube (Schlenk tube), connect a balloon filled with carbon dioxide to the Schlenk tube through the side tube, and wash 3 times, add dodecyldimethylamine caprolactone (5mol % relative to amine), 2-(phenylamino)ethanol (0.25 mmol), polymethylpolysiloxane PMHS (1 mmol) and CH 3 CN (2mL), Schlenk tube heated at 70°C for 12h, cooled to room temperature, released CO in the balloon 2 , EtOAc (10mL) was added to the mixture to quench the reductive reaction, and CH 2 Cl 2 Extract three times, concentrate the organic layer in anhydrous Na 2 SO 4 Drying on , evaporated in vacuo and column chr...

Embodiment 2

[0048] This embodiment provides a method for preparing methylamine, wherein the catalyst used is dodecyldimethylamine caprolactone, and the methylamine is N-benzyl-N-methylaniline. The reaction scheme is as follows:

[0049]

[0050] The preparation method of N-benzyl-N-methylaniline comprises the following steps:

[0051] Take a strictly dry Shrek reaction tube (Schlenk tube), connect a balloon filled with carbon dioxide to the Schlenk tube through the side tube, and wash 3 times, add dodecyldimethylamine caprolactone (5mol % relative to amine), N-benzylaniline (0.25 mmol), polymethylpolysiloxane PMHS (1 mmol) and CH 3 CN (2mL), Schlenk tube heated at 50°C for 10h, cooled to room temperature, released CO in the balloon 2 , EtOAc (10mL) was added to the mixture to quench the reductive reaction, and CH 2 Cl 2 Extract three times, concentrate the organic layer in anhydrous Na 2 SO 4 Drying on , evaporated in vacuo and column chromatography on silica gel with petroleum e...

Embodiment 3

[0055] This example provides a method for preparing methylamine, wherein the catalyst used is dodecyldimethylamine caprolactone, and the methylamine is N,N-dimethyl-[1,1'-diphenyl Base]-2-amine, the reaction scheme of preparing methylamine is as follows:

[0056]

[0057] The preparation method of N,N-dimethyl-[1,1'-diphenyl]-2-amine comprises the following steps:

[0058] Take a strictly dry Shrek reaction tube (Schlenk tube), connect a balloon filled with carbon dioxide to the Schlenk tube through the side tube, and wash 3 times, add dodecyldimethylamine caprolactone (5mol % relative to amine), N-methyl-[1,1'-diphenyl]-2-amine (0.25mmol), polymethylpolysiloxane PMHS (1.2mmol) and CH 3 CN (2mL), Schlenk tube heated at 60°C for 6h, cooled to room temperature, release the CO in the balloon 2 , EtOAc (10mL) was added to the mixture to quench the reductive reaction, and CH 2 Cl 2 Extract three times, concentrate the organic layer in anhydrous Na 2 SO 4 Drying on , evapor...

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Abstract

The invention provides a preparation method of methylamine. The preparation method comprises the following step: preparing methylamine by utilizing an amine methylation reaction, wherein in the aminemethylation reaction, the catalyst is dodecyldimethylamine caprolactone. According to the invention, additives required by the reaction are effectively reduced, and the post-treatment process after the reaction is finished is simplified.

Description

technical field [0001] The invention relates to the technical field of preparing methylamine, in particular to a method for preparing methylamine. Background technique [0002] Methylamine is an important intermediate widely used in the preparation of dyes, natural products and fine chemicals. Traditionally, methylamine is usually prepared from amine using formaldehyde, methyl iodide or dimethyl sulfate as the methylating agent. However, the toxicity and limited substrate scope associated with methylating agents are significant drawbacks of these existing methods. In this regard, from the perspective of sustainable chemistry, a method using CO 2 The synthesis method as the C1 building block becomes a substitute for methylamine among amines and is promising. Carbon dioxide is an abundant and renewable C1 synthon widely used in the synthesis of value-added chemicals. Much effort has been made in the field of carbon dioxide conversion, resulting in a series of valuable chem...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C213/08C07C215/16C07C213/10C07C209/68C07C209/84C07C211/48C07C211/45C07D209/08C07C217/84B01J31/02B01J31/04
CPCC07C213/08C07C213/10C07C209/68C07C209/84C07D209/08B01J31/0279B01J31/04C07C215/16C07C211/48C07C211/45C07C217/84
Inventor 赵继阳杜攀刘姗姗乐振
Owner NANJING XIAOZHUANG UNIV
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