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Methylation method of amine

A methylation and organic amine technology, applied in the field of organic synthesis, can solve the problems of potential safety hazards and limitations of highly toxic reagents, and achieve the effects of high selectivity and yield, more substrates, and low reaction temperature

Active Publication Date: 2019-12-31
Z RIVER GRP LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These highly toxic reagents have potential safety hazards and are quite limited in practical use

Method used

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  • Methylation method of amine

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0035] The preparation method of example 1, composite catalyst, carries out following steps successively

[0036] ①. Weigh 10g of Ni-Al-Mo-Cd-Fe alloy powder into a beaker, the mass fraction of Ni in the alloy powder is 60%, the mass fraction of Al is 38.67%, the mass fraction of Mo is 0.67%, and the mass fraction of Cd is 0.33%, The mass fraction of Fe is 0.33%; then 50 mL of sodium hydroxide solution with a concentration of 5 mol / L is added dropwise to the above alloy powder (dropping time is 20 min), and kept in an ice-water bath (about 0° C.) during the dropping process And magnetic stirring at 120r / min, after the dropwise addition, continue to stir for 30min (in an ice-water bath, 120r / min).

[0037] Explanation: According to the mass fraction notified above, the alloy powder as raw material can be easily obtained according to the known technology.

[0038] 2. Post-processing the reaction product obtained after the stirring reaction, the post-processing is: filtering the...

Embodiment 1

[0041] Embodiment 1, a kind of production method of tetramethylethylenediamine, comprises the steps:

[0042] 1) Add 12g (0.2mol) of ethylenediamine, 25.8g (0.86mol) of paraformaldehyde, and 36g of methanol into the autoclave, then add 0.84g of composite catalyst, replace with nitrogen for 3 times, and feed hydrogen into the autoclave The pressure is controlled at 1.5MPa, the reaction temperature is 50°C, and the reaction time is 9h.

[0043] Note: During the whole reaction process, it is necessary to control the pressure in the autoclave to always be 1.5Mpa by adjusting the amount of hydrogen.

[0044] 2), after the reaction is finished, cool to room temperature, filter, and the filter cake obtained by filtering is washed with deionized water to neutrality, and then stored in water as a recyclable composite catalyst. The obtained filtrate was subjected to atmospheric distillation, and the fraction at 120°C was collected to obtain the product—tetramethylethylenediamine, with ...

Embodiment 2～ Embodiment 9

[0046] Change the molar ratio of ethylenediamine and paraformaldehyde in Example 1, catalyst consumption, reaction time and reaction temperature, all the other are equal to Example 1, respectively obtain Example 2~Example 9, the product obtained---Tetramethyl The yield of ethylenediamine is shown in Table 1 (the purity is all about 99%).

[0047] Table 1

[0048]

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PUM

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Abstract

The invention discloses a methylation method of amine. The method includes: taking hydrogen as a reducing agent, and carrying out methylation reaction on organic amine, paraformaldehyde and a composite catalyst in a solvent; utilizing hydrogen to adjust the pressure of the methylation reaction at (1.5+ / -0.1)Mpa, controlling the temperature of the methylation reaction at 40-60DEG C, and controllingthe time of the methylation reaction at 8-10h; and carrying out post-treatment on the obtained reaction solution to obtain a methylation product of amine. According to the method, the composite catalyst is prepared for catalytic hydrogenation, so that the yield of amine methylation can reach 90% or above, and the byproduct only has water, therefore the method is green and environment-friendly.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a methylation method of organic amines. Background technique [0002] Methyl-substituted amines widely exist in natural products, and have important applications in large chemical industry, fine chemical industry, pharmaceuticals and dyes. [0003] Judging from the domestic and foreign literature reported so far, according to the difference between methylating reagents and reducing agents, they can be mainly divided into the following categories: [0004] 1. Use formaldehyde as a methylating reagent and carboxylic acid as a reducing agent to react. Literature (Synthetic Communications, 2002, 32 (3), 457-465) has reported that formic acid and formaldehyde are used as methylating reagents to react with ethylenediamine, and the reaction temperature is 100°C. This method has a high conversion rate and a single product, but there are problems Because formic acid is oxidi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/60C07C211/10C07C211/35C07C211/48C07C211/27B01J23/887
CPCC07C209/60B01J23/8873C07C2601/14C07C211/10C07C211/35C07C211/48C07C211/27Y02P20/584
Inventor 张超曹忠张华
Owner Z RIVER GRP LTD
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