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Method for preparing hemostatic 6-amino caproic acid

A technology of aminocaproic acid and aminocaproic acid hydrochloride, which is applied in the preparation of organic compounds, chemical instruments and methods, and cyanide reaction preparation, can solve the problems of increased synthesis cost, cumbersome operation, and high risk, and achieve Suitable for large-scale production, mild reaction conditions, and reduced synthesis costs

Inactive Publication Date: 2008-02-20
TIANJIN UNIVERSITY OF TECHNOLOGY
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Problems solved by technology

[0006] In the first method, the 6-aminocaproic acid hydrochloride aqueous solution containing hydrochloric acid is directly passed through the strong acidic cation exchange resin, which needs to be left standing overnight, which takes a long time; without concentration, because it contains a large amount of hydrochloric acid, it is then eluted with ammonia water, and the Standing overnight, the amount of ammonia water is large, time-consuming, and cumbersome to operate; activated carbon decolorization takes nearly an hour, which takes a long time and has a large loss, which increases the operating procedures and increases the synthesis cost.
Resin adsorption is not used in method 2, but the addition of yellow lead powder, aluminum hydroxide, and silver oxide significantly increases the cost; using toxic hydrogen sulfide to remove metal ions is complicated and dangerous

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  • Method for preparing hemostatic 6-amino caproic acid

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Embodiment Construction

[0010] The preparation steps of the present invention are as follows: dissolving caprolactam in 10% hydrochloric acid aqueous solution, heating to reflux, and concentrating to dryness under reduced pressure, so that hydrogen chloride does not remain in the solution to obtain 6-aminocaproic acid hydrochloride. Then the spherical macroporous weakly basic styrene-based anion exchange resin was soaked in distilled water overnight, loaded into a separation column, eluted with 0.8% aqueous ammonia solution, washed with water until neutral, and dissolved in 6-aminocaproic acid hydrochloride. Put it in water, put it into a column, elute with water, collect the eluate, concentrate it to dryness under reduced pressure, add absolute ethanol, precipitate crystals, filter, and dry to obtain 6-aminocaproic acid.

[0011] In the present invention, the weakly basic anion exchange resin is a spherical macroporous weakly basic styrene-based anion exchange resin, and its model is D370 or D301.

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Abstract

The invention discloses a preparation method of 6-aminocaproic acid which is a hemostatic. The preparation method is characterized in that caprolactam is dissolved in diluted hydrochloric acid, heated and refluxed to produce 6-aminocaproic acid hydrochloride which is neutralized by spherical macro-porous styrene type weak alkaline anion exchange resin, thereby acquiring the product after treatment. Compared with other preparation methods, the reaction condition of the method is mild, and metal ion can not be mixed easily, the method is more scientific and rational, the standard of the burn residue required by the original material quality can be realized more easily, white crystal can be obtained from the product without activated carbon decolorizing, the operation is simple, the synthesizing cost is reduced and mass production of the technology is more suitable.

Description

【Technical field】 [0001] The invention relates to the technical field of organic synthesis, in particular to a preparation method of hemostatic drug 6-aminocaproic acid. 【Background technique】 [0002] 6-aminohexanoic acid (6-Aminohexanoic acid), molecular formula: C 6 h 13 NO 2 , is a hemostatic agent widely used at home and abroad at present. It has obvious curative effect on certain severe bleeding caused by increased fibrinolytic activity. Tract bleeding and obstetrics and gynecology hemorrhagic disorders. In the prior art, the following patents and documents relate to the preparation method of 6-aminocaproic acid, such as U.S.Pat2 453,234; Org.syn.Coll.vol II, 28 (1943); Org.syn.Coll.Vol IV, 39 (1963); Hebei Chemical Industry, 2003, April, 24; Organic Synthesis Code (Edited by Fan Nengting), P394, etc. The above-mentioned patented technology is related to the literature method, and its synthetic route mainly contains the following two methods: [0003] Method 1: U...

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C229/08C07C227/22
Inventor 陈宝泉李彩文黄玉平包梦静侯晓红
Owner TIANJIN UNIVERSITY OF TECHNOLOGY
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