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A kind of 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: 2022-07-29
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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  • A kind of preparation method of methylamine
  • A kind of preparation method of methylamine
  • A kind of 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, and the methylamine is 2-(methyl(phenyl)amino)ethanol to prepare methylamine. The reaction scheme for the amine is shown below:

[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, wash it three times, and add dodecyldimethylamine caprolactone (5 mol) in turn. % 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, CO released from balloon 2 , EtOAc (10 mL) was added to the mixture to quench the reduction reaction, and CH 2 Cl 2 Extracted three times, the concentrated organic layer was washed with anhydrous Na 2 S...

Embodiment 2

[0048] This embodiment provides a method for preparing methylamine, wherein the catalyst used is dodecyldimethylamine caprolactone, the methylamine is N-benzyl-N-methylaniline, and the method for preparing methylamine is The reaction route 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, wash it three times, and add dodecyldimethylamine caprolactone (5 mol) in turn. % 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, CO released from balloon 2 , EtOAc (10 mL) was added to the mixture to quench the reduction reaction, and CH 2 Cl 2 Extracted three times, the concentrated organic layer was washed with anhydrous Na 2 SO 4 It was dried on ...

Embodiment 3

[0055] This embodiment provides a method for preparing methylamine, wherein the catalyst used is dodecyldimethylamine caprolactone, and the methylamine is N,N-dimethyl-[1,1'-diphenylene] base]-2-amine, the reaction scheme for 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, wash it three times, and add dodecyldimethylamine caprolactone (5 mol) in turn. % relative to amine), N-methyl-[1,1'-diphenyl]-2-amine (0.25 mmol), polymethylpolysiloxane PMHS (1.2 mmol) and CH 3 CN (2mL), Schlenk tube heated at 60°C for 6h, cooled to room temperature, CO released from balloon 2 , EtOAc (10 mL) was added to the mixture to quench the reduction reaction, and CH 2 Cl 2 Extracted three times, the concentrated organic layer was washed with ...

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Abstract

The invention provides a preparation method of methylamine, which is to prepare methylamine by amine methylation reaction; in the amine methylation reaction, the catalyst is dodecyldimethylamine caprolactone . The invention effectively reduces the additives required for the reaction, and is beneficial to simplify the post-processing process after the reaction is completed.

Description

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

Claims

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Application Information

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Patent Type & Authority Patents(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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