Preparation method of 2-methoxy ethylamine

A technology of methoxyethylamine and methoxyethylamine hydrochloride, which is applied in the preparation of 2-methoxyethylamine, organic chemistry, and the field of 2-methoxyethylamine, can solve the problem of undetected 2- Problems such as methoxyethylamine products, to achieve the effects of low production cost, less three wastes, and less environmental pollution

Inactive Publication Date: 2014-07-23
SHANGHAI TBBMED CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

We have verified the reaction, and it is not as reported in the literature. Even if NaH is used as the raw material, it is still an N-methylated product, and 1H NMR did not detect the 2-methoxyethylamine product.

Method used

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  • Preparation method of 2-methoxy ethylamine
  • Preparation method of 2-methoxy ethylamine
  • Preparation method of 2-methoxy ethylamine

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Embodiment 1

[0029] step 1:

[0030] Toluene (500mL), benzaldehyde (70.0g, 0.660mol) and ethanolamine (40.3g, 0.660mol) were successively added to a 1L single-necked flask, refluxed for azeotropic dehydration for 16h, and the reaction was detected by GC to obtain the compound 2-benzylidene The toluene solution of amine ethanol (formula II) was directly used in the next step without purification.

[0031] Step 2:

[0032] The reaction solution in the previous step was transferred to a 1L three-necked flask filled with 50% NaOH aqueous solution (211g, 2.64mol), and under mechanical stirring, dimethyl carbonate (120g, 1.32mol) was added dropwise. Reaction for 2h, GC detects that the reaction is over, add 350mL water to dilute, separate the organic phase, extract the aqueous phase with toluene (100mL X2), combine the organic phase to obtain a toluene solution of the compound N-benzyl-2-methoxyl-ethanolamine, without Purification was used directly in the next reaction.

[0033] Step 3:

[...

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Abstract

The invention relates to a preparation method of 2-methoxy ethylamine. The preparation method comprises the following steps: preparing a benzyl imine intermediate; preparing an N-benzyl alkenyl-2-methoxy ethylamine intermediate; preparing a 2-methoxy ethylamine hydrochloride aqueous solution; preparing a 2-methoxy ethylamine solution; and desolventizing the 2-methoxy ethylamine solution and rectifying, and collecting fractions at 82-85 DEG C, wherein the total yield is 56-84%, the purity is greater than 99.7% and the water content is less than 0.2%. According to the preparation method provided by the invention, by using cheap ethanol amine as a raw material, the final product 2-methoxy ethylamine can be obtained by the following steps: carrying out azeotropic dehydration with benzaldehyde to generate aldimine; then, methylating under an alkaline condition; and removing protection and alkalizing and rectifying. The preparation method is low in production cost, fewer in three wastes, safe, easy to operate and suitable for industrialization.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to organic chemistry, in particular to 2-methoxyethylamine, and specifically to a preparation method of 2-methoxyethylamine. Background technique [0002] 2-Methoxyethylamine (formula V) is a very important chemical raw material, widely used in the synthesis of pharmaceutical and pesticide intermediates, such as: document WO2014 / 136 report compound (formula VI) is a potential potassium ion Regulators, used to treat and alleviate various diseases related to potassium ion channels; document WO2013012723 reports that compounds (formula VII) are used as tankyrase inhibitors for the treatment of diseases such as cancer; [0003] [0004] At present, regarding the synthesis of 2-methoxyethylamine, it is produced industrially by high-temperature dehydration of ethylene glycol monomethyl ether and ammonia under the catalysis of nickel or alumina, or by hydrogenation of methoxyacetonitril...

Claims

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Application Information

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IPC IPC(8): C07C213/08C07C217/08
Inventor 高峰皮红军袁新曾赛兰
Owner SHANGHAI TBBMED CO LTD
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