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Preparation method for glycinamide hydrochloride

A technology of glycinamide and aminoacetonitrile hydrochloride, applied in the chemical industry, can solve the problems of slow reaction speed, low yield, large amount of ammonium carbonate, etc., and achieve the effects of less by-products, high yield and mild reaction conditions

Active Publication Date: 2013-08-28
ANHUI ANLITAI BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the production methods of glycinamide hydrochloride mainly include the chloroacetamide method and the methyl chloroacetate method: the chloroacetamide method mainly uses a large amount of ammonia as a solvent. This method has a low degree of industrialization and is mainly used in laboratory production. The methyl chloroacetate method is divided into ammonia water solvent method and methanol solvent method again, and wherein ammonia water solvent method needs a large amount of ammonia water as solvent equally, and the used catalyst ammonium carbonate consumption of methanol solvent method is very large, can produce a large amount of carbon dioxide and can't handle , and the reaction temperature is difficult to control smoothly
In the above-mentioned prior art, the production method of glycinamide hydrochloride either has a slow reaction speed, is difficult to control the entire process conditions smoothly, or has a low yield and high production cost. Therefore, a kind of glycine with mild reaction conditions and high yield is sought. The preparation method of amide hydrochloride is of great significance

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 1) Preparation of aminoacetonitrile amine hydrochloride:

[0024] Add 35.4g of ammonium chloride, 46ml of 30% ammonia water, 110.2g of 28% sodium cyanide solution and 160ml of water into a 1000ml three-necked flask, stir magnetically, and drop 55ml of 35% formaldehyde was added dropwise in about 1.5 hours, and the color was detected by TLC in an iodine tank, kept at 15°C for 8 hours, and then extracted three times with 50ml of 99.0% 1,2-dichloroethane, and the extracted The organic phases were combined, fully dried with excess anhydrous sodium sulfate, then passed hydrogen chloride gas at room temperature until the pH was 4, filtered with suction, and finally rinsed with acetone to obtain 46.89 g of approximately white solid aminoacetonitrile hydrochloride. The rate is 80.5%, and the melting point is 170-176°C.

[0025] 2) Preparation of glycinamide hydrochloride:

[0026] Add 148ml of isopropanol with a concentration of 99.0% (the amount of the substance is 1.94mol) ...

Embodiment 2

[0028] 1) Preparation of aminoacetonitrile amine hydrochloride:

[0029] Add 39.8g of ammonium chloride, 49ml of ammonia water (25%), 110.2g of sodium cyanide solution (28%) and 160ml of water into a 1000ml three-necked flask, stir magnetically, and add dropwise 60ml of formaldehyde (35%) at 10°C , the dropwise addition was completed in about 1.5 hours, and the iodine tank was detected by TLC for color development, kept at 20°C for 4 hours, then extracted three times with 55ml of 1,2-dichloroethane (99.0%), and the organic phase obtained by extraction Combined, fully dried with excess anhydrous sodium sulfate, then passed hydrogen chloride gas at room temperature until the pH was 3, filtered with suction, and finally rinsed with acetone to obtain 43.9 g of approximately white solid aminoacetonitrile hydrochloride, with a yield of 75.4% , melting point 171 ~ 176 ° C.

[0030] 2) Preparation of glycinamide hydrochloride:

[0031] Add 92ml of isopropanol (99.0%) (the amount of ...

Embodiment 3

[0033] 1) Preparation of aminoacetonitrile amine hydrochloride:

[0034] Add 33.2g of ammonium chloride, 49ml of ammonia water (30%), 110.2g of sodium cyanide solution (28%) and 160ml of water into a 1000ml three-necked flask, stir magnetically, and add 54.5ml of formaldehyde (35% ), the dropwise addition was completed in about 1.5 hours, and the iodine cylinder was detected by TLC for color development, kept at room temperature for 6 hours, then extracted three times with 55ml of 1,2-dichloroethane (99.0%), and the organic phases obtained by the extraction were combined, Fully dry with excess anhydrous sodium sulfate, then pass hydrogen chloride gas at room temperature until the pH is 4, filter with suction, and finally rinse with acetone to obtain 47.5 g of approximately white solid aminoacetonitrile hydrochloride, with a yield of 80.1.7% , melting point 170 ~ 173 ℃.

[0035] 2) Preparation of glycinamide hydrochloride:

[0036] Add 120ml of isopropanol (99.0%) (the amount...

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Abstract

The invention discloses a preparation method for glycinamide hydrochloride. The preparation method for glycinamide hydrochloride comprises the following steps of: a) dissolving glycinonitrile hydrochloride in isopropanol; b) heating to 50-70 DEG C; c) charging dried hydrogen chloride gas until the dried hydrogen chloride gas is saturated; d) insulating heat for 4-5 hours; e) cooling to room temperature; and f) performing suction filtration to obtain glycinamide hydrochloride. Compared with the prior art. The preparation method for glycinamide hydrochloride is moderate in reaction conditions, high in yield, and few in by-products.

Description

technical field [0001] The invention relates to the technical field of chemical engineering, in particular to a preparation method of a pharmaceutical intermediate. Background technique [0002] Glycine amide hydrochloride is one of the important compounds in amide derivatives, and it is widely used in the preparation of medicine and pesticide as an organic synthesis intermediate. At present, the production methods of glycinamide hydrochloride mainly include the chloroacetamide method and the methyl chloroacetate method: the chloroacetamide method mainly uses a large amount of ammonia as a solvent. This method has a low degree of industrialization and is mainly used in laboratory production. The methyl chloroacetate method is divided into ammonia water solvent method and methanol solvent method again, and wherein ammonia water solvent method needs a large amount of ammonia water as solvent equally, and the used catalyst ammonium carbonate consumption of methanol solvent meth...

Claims

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Application Information

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IPC IPC(8): C07C237/06C07C231/06
Inventor 马云峰吴梅
Owner ANHUI ANLITAI BIOTECH CO LTD
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