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Method for preparing methylamino-acetonitrilehydrochlorate

A technology of methylaminoacetonitrile hydrochloride and aminoacetonitrile hydrochloride, which is applied in the field of preparation of methylaminoacetonitrile hydrochloride, can solve the problems of high cost, cumbersome operation, and large investment in equipment, and achieve the effect of inhibiting hydrolysis

Active Publication Date: 2009-04-08
太仓市茜泾化工有限公司
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Problems solved by technology

[0006] 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 low, and the cost is high, which is uneconomical; while the hydroxyacetonitrile method has a reaction step of Long, cumbersome operation, large equipment investment, and high cost; the sodium cyanide method has the advantage of simple operation, but the yield is low, only about 50%

Method used

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Embodiment Construction

[0013] The present invention will be described in detail below in conjunction with a specific embodiment, but not limited to this embodiment.

[0014] A preparation method of methylaminoacetonitrile hydrochloride, comprising the steps of:

[0015] (1) Preparation of methylaminoacetonitrile: 67.5g of methylamine hydrochloride, 120g of 30% formaldehyde and 4.9g of 3-mercaptopropionic acid were put into a four-neck flask, stirred for 30 minutes, cooled to below 0°C, and slowly 163 g of 30% aqueous solution of sodium cyanide was added dropwise, the dropping temperature was controlled at 0° C., and the dropping time was controlled at 2 to 3 hours. After the dropwise addition, stir for 30 minutes below 0°C, then stand still for 30 minutes, separate layers, and separate the oil layer from the upper layer, which is methylaminoacetonitrile.

[0016] (2) Preparation of methylaminoacetonitrile hydrochloride: put 50 g of absolute ethanol and 50 g of methylaminoacetonitrile into a four-ne...

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Abstract

The invention relates to a preparation method for methylamino-acetonitrile hydrochlorate. The preparation method comprises the following steps: (1) using methylamine hydrochlorate, sodium cyanide and formaldehyde as reaction raw materials, and performing reaction in the presence of a catalyst to generate methylamino-acetonitrile; (2) causing the methylamino-acetonitrile to react with hydrochloric acid to generate the methylamino-acetonitrile hydrochlorate, wherein in step (1), below zero DEG C, using 3-hydrosulfuryl propanoic acid as a catalyst with the dose of 0.9 to 1.1 times of the sodium cyanide. The preparation method not only has simple operation, but also has high yield and low cost, and is suitable for industrial production.

Description

technical field [0001] The invention relates to a preparation method of methylaminoacetonitrile hydrochloride. Background technique [0002] In the prior art, the method for synthesizing aminoacetonitrile mainly contains following several kinds: [0003] Sodium cyanide method: use amine, sodium cyanide, formaldehyde, react and synthesize in the presence of magnesium salts such as magnesium chloride or magnesium sulfate; [0004] Liquid hydrocyanic acid method: use amine, formaldehyde, and liquid hydrocyanic acid as raw materials, add formaldehyde and hydrocyanic acid dropwise at the same time, react, extract and crystallize to obtain aminoacetonitrile, with a yield of 80-95% and a content of 92-98%; [0005] Hydroxyacetonitrile method: Use hydrocyanic acid and formaldehyde to react to generate hydroxyacetonitrile, and then condense with amine to obtain aminoacetonitrile. [0006] Among the above-mentioned methods, although the liquid hydrocyanic acid method has a higher yi...

Claims

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Application Information

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IPC IPC(8): C07C255/25C07C253/00
Inventor 吴健明
Owner 太仓市茜泾化工有限公司
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