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A kind of preparation method of methylaminoacetonitrile hydrochloride

A technology of methylaminoacetonitrile hydrochloride and methylamine hydrochloride, which is applied in the field of preparation of methylaminoacetonitrile hydrochloride, can solve the problems of high operation risk, long reaction steps, large equipment investment, etc., and achieve low operation risk factor , low cost, less by-products

Active Publication Date: 2022-05-24
太仓市茜泾化工有限公司
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  • Abstract
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Problems solved by technology

[0003] But among the above-mentioned methods, although the liquid hydrocyanic acid method has a higher yield, the operation risk is large. In order to obtain the liquid hydrocyanic acid, a refrigeration system is needed, and the equipment investment is small, the cost is high, and it is uneconomical; while the hydroxyacetonitrile method reacts The steps are long, the operation is complicated, the equipment investment is large, and the cost is high; the sodium cyanide method has the advantage of simple operation, but the yield is low, only about 50%, so we have proposed a kind of methylaminoacetonitrile hydrochloride. preparation method to solve the above problems

Method used

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  • A kind of preparation method of methylaminoacetonitrile hydrochloride
  • A kind of preparation method of methylaminoacetonitrile hydrochloride
  • A kind of preparation method of methylaminoacetonitrile hydrochloride

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Embodiment 1

[0032] see figure 1 , the present invention provides the following technical solutions: a preparation method of methylaminoacetonitrile hydrochloride, comprising the following steps:

[0033] S1: Weigh 1200㎎ methylamine aqueous solution, 1150㎎ hydrochloric acid, 1325㎎ formaldehyde, 35㎎ acetic acid, 1850㎎ sodium cyanide aqueous solution, 635㎎ anhydrous ethanol and 545㎎ hydrochloric acid ethanol for use;

[0034] S2: Pour the 1200㎎ methylamine aqueous solution weighed in S1 into the flask, then heat it, then add the 1150㎎ hydrochloric acid weighed in S1 into the flask, and use a glass rod to stir and mix, so that the reaction can generate Methylamine hydrochloride solution;

[0035] S3: Pour the methylamine hydrochloride solution prepared in S2 into a distillation flask, carry out distillation treatment, remove 65% of the water, then cool to room temperature, and then put the solution cooled to room temperature into a centrifugal reducer Drying under reduced pressure is carrie...

Embodiment 2

[0047] see figure 1 , the present invention provides the following technical solutions: a preparation method of methylaminoacetonitrile hydrochloride, comprising the following steps:

[0048] S1: Weigh 1200㎎ methylamine aqueous solution, 1150㎎ hydrochloric acid, 1325㎎ formaldehyde, 35㎎ acetic acid, 1850㎎ sodium cyanide aqueous solution, 635㎎ anhydrous ethanol and 545㎎ hydrochloric acid ethanol for use;

[0049] S2: Pour the 1200㎎ methylamine aqueous solution weighed in S1 into the flask, then heat it, then add the 1150㎎ hydrochloric acid weighed in S1 into the flask, and use a glass rod to stir and mix, so that the reaction can generate Methylamine hydrochloride solution;

[0050] S3: Pour the methylamine hydrochloride solution prepared in S2 into a distillation flask, carry out distillation treatment, remove 65% of the water, then cool to room temperature, and then put the solution cooled to room temperature into a centrifugal reducer Drying under reduced pressure is carrie...

Embodiment 3

[0059] see figure 1 , the present invention provides the following technical solutions: a preparation method of methylaminoacetonitrile hydrochloride, comprising the following steps:

[0060] S1: Weigh 1200㎎ methylamine aqueous solution, 1150㎎ hydrochloric acid, 1325㎎ formaldehyde, 35㎎ acetic acid, 1850㎎ sodium cyanide aqueous solution, 635㎎ anhydrous ethanol and 545㎎ hydrochloric acid ethanol for use;

[0061] S2: Pour the 1200㎎ methylamine aqueous solution weighed in S1 into the flask, then heat it, then add the 1150㎎ hydrochloric acid weighed in S1 into the flask, and use a glass rod to stir and mix, so that the reaction can generate Methylamine hydrochloride solution;

[0062] S3: Pour the methylamine hydrochloride solution prepared in S2 into a distillation flask, carry out distillation treatment, remove 65% of the water, then cool to room temperature, and then put the solution cooled to room temperature into a centrifugal reducer Drying under reduced pressure is carrie...

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Abstract

The invention belongs to the technical field of methylaminoacetonitrile hydrochloride, in particular to a method for preparing methylaminoacetonitrile hydrochloride, comprising the following steps: S1: weighing an appropriate amount of methylamine aqueous solution, hydrochloric acid, formaldehyde, acetic acid, and sodium cyanide aqueous solution , absolute ethanol and hydrochloric acid ethanol for use; S2: Pour the methylamine aqueous solution weighed in S1 into the flask, then heat, then add the hydrochloric acid weighed in S1 into the flask, and use a glass rod to stir Mix, so that it can react to generate methylamine hydrochloride solution. Compared with the prior art, the present invention has a reaction yield of more than 75%, a target product methylaminoacetonitrile hydrochloride content of more than 98%, mild reaction conditions, less by-products, simple process, simple operation and low cost , and the operation risk factor is low, so it is more suitable for industrial production.

Description

technical field [0001] The invention relates to the technical field of methylaminoacetonitrile hydrochloride, in particular to a preparation method of methylaminoacetonitrile hydrochloride. Background technique [0002] Methylaminoacetonitrile hydrochloride can be used as an intermediate in pharmaceutical and chemical synthesis. In the prior art, the methods for synthesizing aminoacetonitrile mainly include the following: sodium cyanide method: adopt amine, sodium cyanide, formaldehyde, react and synthesize in the presence of magnesium salts such as magnesium chloride or magnesium sulfate; liquid hydrocyanic acid method: use Amine, formaldehyde and liquid hydrocyanic acid are used as raw materials, and formaldehyde and hydrocyanic acid are added dropwise at the same time, and aminoacetonitrile is obtained through reaction and extraction crystallization, with a yield of 80-95% and a content of 92-98%; hydroxyacetonitrile method: using hydrocyanic acid It first reacts with fo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C253/00C07C253/30C07C253/34C07C255/25C07C209/74C07C209/84C07C211/04B01F35/32B01F27/90
CPCC07C253/00C07C253/30C07C253/34C07C209/74C07C209/84B01F27/90B01F35/4111B01F35/43B01F2101/2204C07C211/04C07C255/25
Inventor 秦正浩
Owner 太仓市茜泾化工有限公司
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