A kind of preparation method of L-hydroxyproline single crystal

A technology of hydroxyproline and single crystal, which is applied in the field of preparation of L-hydroxyproline single crystal, which can solve the problems of randomness, difficulty in large-scale industrial production, and low quality of ordinary crystal products, and achieve low solvent pollution and low pollution , easy to transport and store, no discoloration effect

Active Publication Date: 2019-10-29
HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The present invention aims at the problems of low quality common crystal products existing in the preparation process of L-hydroxyproline in the prior art, large randomness in production and difficulty in large-scale industrial production, etc., and provides a single crystal of L-hydroxyproline preparation method

Method used

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  • A kind of preparation method of L-hydroxyproline single crystal
  • A kind of preparation method of L-hydroxyproline single crystal
  • A kind of preparation method of L-hydroxyproline single crystal

Examples

Experimental program
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Effect test

Embodiment 1

[0034] Weigh 13.11g of ordinary L-hydroxyproline powder and 15.20g of ethylene glycol monomethyl ether in a ratio of 1:2; mix and stir at 75°C for 55 minutes to make L-hydroxyproline in ethylene Alcohol monomethyl ether is completely dissolved; at the same time, 6wt% tetrabutylammonium bromide / ethylene glycol eutectic solvent 0.79g and 1.5wt% L-hydroxyproline based on the mass of L-hydroxyproline powder are added Amino acid single crystal seed crystal 0.20g; mixed and stirred for 6 min under the condition of keeping constant temperature, the reaction was stopped; the temperature of the solution was reduced in the range of 75-65℃ according to 0.3℃ / min, and 0.5℃ in the range of 65-40℃ Cool down at a temperature of 1.5°C / min in the range of 40-20°C, and then keep the temperature at 20°C for a period of time until no L-hydroxyproline single crystal precipitates. Filtration, washing, and vacuum drying to obtain white needle-like L-hydroxyproline single crystals. The entire crystall...

Embodiment 2

[0036] Weigh 13.11g of ordinary L-hydroxyproline powder and 22.80g of ethylene glycol monomethyl ether, mix and stir at 65°C for 60 minutes until completely dissolved; while maintaining constant temperature, add tetraethylammonium chloride / glycerol Alcohol eutectic solvent 0.79g and L-hydroxyproline single crystal seed crystal 0.20g; mixed and stirred for 6min, the reaction was stopped; at 65-55℃, the temperature was lowered at 0.4℃ / min, and at 55-40℃, it was at 0.8 Cool down at a temperature of 2°C / min in the range of 40-20°C, and then keep the temperature at 20°C for a period of time until no L-hydroxyproline single crystal is precipitated. Filtration, washing, and vacuum drying to obtain white needle-like L-hydroxyproline single crystals. The entire crystallization process takes about 3h, and the filtered mother liquor is reused. The obtained L-hydroxyproline single crystal was placed in the air for 24 hours without agglomeration. The moisture absorption was determined to b...

Embodiment 3

[0038] Weigh 26.22g of ordinary L-hydroxyproline powder and 45.60g of ethylene glycol monomethyl ether, mix and stir at 50℃ for 80min to completely dissolve; add tetramethylammonium bromide / glycerol low at 50℃ 1.75g ​​of eutectic solvent and 0.40g of L-hydroxyproline single crystal seed crystal; mixed and stirred for 8 minutes and then stopped the reaction; in the range of 50-45℃, the temperature will be reduced according to 0.5℃ / min, and in the range of 45-40℃ according to 0.6℃ / The temperature is lowered in minutes, and the temperature is lowered at 1.5°C / min in the range of 40-20°C, and then kept at 20°C for aging for a period of time until no L-hydroxyproline single crystal is precipitated. Filtration, washing, and vacuum drying to obtain white needle-like L-hydroxyproline single crystals. The entire crystallization process takes about 3h, and the filtered mother liquor is reused. The obtained L-hydroxyproline single crystal was placed in the air for 24 hours without agglo...

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Abstract

The invention belongs to the field of chemistry, and particularly relates to a preparation method of an L-hydroxyproline monocrystal. The preparation method comprises the following steps: (1) weighing L-hydroxyproline powder and ethylene glycol monomethyl ether according to proportions; (2) mixing and stirring for 15 to 120 minutes under 30 to 85 DEG C, and enabling L-hydroxyproline to be completely dissolved in the ethylene glycol monomethyl ether; (3) simultaneously adding a quaternary ammonium salt eutectic solvent and an L-hydroxyproline monocrystal seed; (4) stopping reacting after mixing and stirring for 5 to 10 minutes under the condition of keeping a constant temperature; (5) gradually cooling to 20 to 30 DEG C by adopting programmed cooling, and then aging for a certain time until no L-hydroxyproline monocrystal is separated out; (6) filtering, washing, and vacuum drying, thus obtaining a white needle-like L-hydroxyproline monocrystal. By adopting the technical scheme of the invention, an obtained L-hydroxyproline monocrystal product is high in quality, is not easy to absorb moisture and deliquesce, has no color change and is good in thermal stability; the technical operating conditions are mild, volume production efficiency is high, the period is short, a solvent is difficult to volatize, the pollution is small, cyclic utilization can be realized, and three wastes are not generated.

Description

Technical field [0001] The invention belongs to the field of chemistry, and specifically relates to a preparation method of L-hydroxyproline single crystal. Background technique [0002] L-Hydroxyproline (C 5 H 9 NO 2 , Structural formula such as figure 1 Shown), an important imino-neutral amino acid, is an important component of collagen and has the most content. [0003] L-Hydroxyproline was obtained from gelatin by Fischer in 1902, but it did not receive attention for a long time. In recent years, people have gradually discovered that L-hydroxyproline is an important component of mammalian collagen and has many important physiological functions and unique biological activities. The research and development of L-hydroxyproline has attracted the attention of industries such as biology, pharmacy, food and cosmetics. The content of L-hydroxyproline is an important indicator for detecting physiological behaviors such as collagen metabolism, bone resorption, cancer metastasis in the...

Claims

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Application Information

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Patent Type & AuthorityPatents(China)
IPC IPC(8): C07D207/16
CPCC07B2200/13C07D207/16
Inventor任红威俞磊连少翰段二红李雪牛建瑞
OwnerHEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY