CN102850242A - Preparation method of guanidine propionic acid nitrate - Google Patents
Preparation method of guanidine propionic acid nitrate Download PDFInfo
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- CN102850242A CN102850242A CN 201110174945 CN201110174945A CN102850242A CN 102850242 A CN102850242 A CN 102850242A CN 201110174945 CN201110174945 CN 201110174945 CN 201110174945 A CN201110174945 A CN 201110174945A CN 102850242 A CN102850242 A CN 102850242A
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- propionic acid
- guanidine radicals
- preparation
- nitrate
- radicals propionic
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Abstract
A preparation method of guanidine propionic acid nitrate includes uniformly stirring guanidino propionic acid with water, dropwise adding nitric acid, with the temperature controlled at 20 DEG C. to 60 DEG C., for 10 minutes, holding temperature, stirring for 20 minutes, cooling to precipitate solid, filtering and drying to obtain the guanidino propionic acid nitrate. The liquid after filtration is used as the mother liquor in the production cycle. The raw materials used by the present invention include the food grade guanidino propionic acid, and the chemical reagent grade nitric acid, so that the produced guanidino propionic acid nitrate product has few impurities, good quality, and purity of more than 99% without recrystallization, so as to ensure quality, save process and production time and improve production efficiency. The invention utilizes the recycled mother liquor to improve yield, with the product yield reaching more than 98%, and reduces the cost. The present invention is low-cost, simple in preparation process and non-polluting, and is free of byproduct and suitable for industrial production.
Description
Technical field
The present invention relates to the preparation method of a seed amino acid nitrate, specifically the preparation method of guanidine radicals propionic acid nitrate.
Background technology
Amino acid is the base substance that consists of the Animal nutrition desired protein.General people self generate or can obtain to satisfy by food each seed amino acid of somagenic need.But in the situation that special as human infantile period, in the situation that sick, injured or large amount of exercise is taken exercise, for growth needs, recover the balance of various metabolism in the body, strengthening immunity and sportsmen need to regain one's strength as early as possible, increase muscle strength, just need extra each seed amino acid that replenishes.
The guanidine radicals propionic acid is a kind of amino acid that contains guanidine radicals, is the endogenous metabolism product in human body and the animal body, and metabolic disturbance be treated and be prevented to the guanidine radicals propionic acid can, hyperglycemia, hyperinsulinemia, Regular Insulin insensitive, hyperlipidemia, hyperamylasemia, the symptoms such as obesity.The guanidine radicals propionic acid is improved human body endurance as foodstuff additive simultaneously, the effect of lasting force and motion capacity.
Because the solubleness of amidates in water is more much larger than amino acid, it is transformed into amino acid at last through effects such as oxydase in vivo, compares to take directly that amino acid is easier to be absorbed by health.The amount that absorbs is more.So amino acid is usually all made amidates and is taken, and generally makes the amino acid salts hydrochlorate more.Recently U.S. parties concerned research discovery, amino acid whose nitrate more is conducive to amino acid absorption in vivo, therefore the guanidine radicals propionic acid is made into guanidine radicals propionic acid nitrate and takes, and will more easily change into the guanidine radicals propionic acid, is absorbed by health.Dosage can be less when it used, and oral absorption efficient can be higher.
Summary of the invention
The present invention provides a kind of preparation method of guanidine radicals propionic acid nitrate in order to access the guanidine radicals propionate compound that more easily changes into the guanidine radicals propionic acid in human body.
The present invention is that the technical scheme that the technical problem that exists in the above-mentioned technology of solution is taked is:
The preparation method of a kind of guanidine radicals propionic acid nitrate of the present invention is as follows: guanidine radicals propionic acid and water stir, drip nitric acid, the control temperature dropwises after 10 minutes at 20 ℃～40 ℃, continued insulated and stirred 20 minutes, then the solid of guanidine radicals propionic acid nitrate is separated out in cooling.Liquid after the filtration recycles aborning as mother liquor.
The mol ratio of guanidine radicals propionic acid and nitric acid is 1: 1～1.1, and the ratio of guanidine radicals propionic acid and water is 1g: 2ml.
The feed liquid cooling temperature is≤10 ℃.
Advantage and positively effect that the present invention has are: the raw material that the present invention adopts is the guanidine radicals propionic acid of food grade and the nitric acid of chemical reagent-grade, so the guanidine radicals propionic acid nitrate product impurity of producing is few, quality is good, just reach more than 99% without recrystallization purity, both guaranteed quality, save again operation and production time, improved production efficiency.The present invention utilizes Recycling Mother Solution to use, and has improved yield, and the yield of product is reached more than 98%, has reduced cost, has also saved valuable water resources.Preparation method's technique of the present invention rationally, simply, and is pollution-free, and no coupling product is fit to industrialized production.
Embodiment
Solubleness among the present invention in the guanidine radicals propionic acid water is less, need add a certain amount of water during reaction, and water is deionized water, to guarantee the quality of product.Below the narration in just referred to as water.The ratio of guanidine radicals propionic acid and water is 1g: 2ml.
The mol ratio of guanidine radicals propionic acid and nitric acid should be 1: 1 among the present invention, but for the guanidine radicals propionic acid is reacted completely, nitric acid dosage should be more bigger than guanidine radicals propionic acid.
Liquid after the present invention will filter is recycled as mother liquor.Owing to also having minute quantity not have the guanidine radicals propionic acid nitrate of crystallization in the liquid after filtering out, so when it was used for next step production, the crystallization that produces in the feed liquid can both be separated out more than 98%, has greatly improved actual recovery, has saved simultaneously valuable water resources.Quality for fear of masterbatch becomes in recycling process greatly, should material be taken out clean when discharging as far as possible.
For further understanding summary of the invention of the present invention, Characteristic, hereby exemplify following examples:
Embodiment 1
Take by weighing guanidine radicals propionic acid 13.1g (0.1mol) and put into reaction flask, add entry 26.2ml, stir, drip 65% nitric acid 10g (0.1mol), the control temperature dropwised at 25 ℃ in 10 minutes, continued insulated and stirred 20 minutes.Solution is clarified gradually, then is cooled to 5 ℃, separates out the solid of guanidine radicals propionic acid nitrate.After filtration, get guanidine radicals propionic acid nitrate finished product after the drying.Liquid after the filtration recycles aborning as mother liquor.
Embodiment 2
Take by weighing guanidine radicals propionic acid 13.1g (0.1mol) and put into reaction flask, add mother liquor 26ml, stir, drip 65% nitric acid 10g (0.1mol), the control temperature dropwised at 33 ℃ in 10 minutes, continued insulated and stirred 20 minutes.Solution is clarified gradually, then is cooled to 10 ℃, separates out the solid of guanidine radicals propionic acid nitrate.After filtration, get guanidine radicals propionic acid nitrate finished product after the drying.Liquid after the filtration recycles aborning as mother liquor.
Embodiment 3
Take by weighing guanidine radicals propionic acid 13.1g (0.1mol) and put into reaction flask, add mother liquor 26ml, stir, drip 65% nitric acid 10g (0.1mol), the control temperature dropwised at 40 ℃ in 10 minutes, continued insulated and stirred 20 minutes.Solution is clarified gradually, then is cooled to 0 ℃, separates out the solid of guanidine radicals propionic acid nitrate.After filtration, get guanidine radicals propionic acid nitrate finished product after the drying.Liquid after the filtration recycles aborning as mother liquor.
Claims (4)
1. the preparation method of a guanidine radicals propionic acid nitrate, it is characterized in that the preparation method is as follows: guanidine radicals propionic acid and water are stirred, drip nitric acid, the control temperature is at 20 ℃～40 ℃, dropwise after 10 minutes, continued insulated and stirred 20 minutes, then solid is separated out in cooling, get guanidine radicals propionic acid nitrate finished product after filtration, the drying, the liquid after the filtration recycles aborning as mother liquor.
2. the preparation method of guanidine radicals propionic acid nitrate according to claim 1, the mol ratio that it is characterized in that guanidine radicals propionic acid and nitric acid is 1: 1～1.1.
3. the preparation method of guanidine radicals propionic acid nitrate according to claim 1, the ratio that it is characterized in that guanidine radicals propionic acid and water is 1g: 2ml.
4. the preparation method of guanidine radicals propionic acid nitrate according to claim 1 is characterized in that the feed liquid cooling temperature is≤10 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110174945 CN102850242A (en) | 2011-06-27 | 2011-06-27 | Preparation method of guanidine propionic acid nitrate |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201110174945 CN102850242A (en) | 2011-06-27 | 2011-06-27 | Preparation method of guanidine propionic acid nitrate |
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| CN102850242A true CN102850242A (en) | 2013-01-02 |
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| CN 201110174945 Pending CN102850242A (en) | 2011-06-27 | 2011-06-27 | Preparation method of guanidine propionic acid nitrate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108472269A (en) * | 2015-08-25 | 2018-08-31 | 睿治尼斯公司 | With the pharmaceutically acceptable β of improved property-guanidinopropionic acid salt and application thereof |
-
2011
- 2011-06-27 CN CN 201110174945 patent/CN102850242A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108472269A (en) * | 2015-08-25 | 2018-08-31 | 睿治尼斯公司 | With the pharmaceutically acceptable β of improved property-guanidinopropionic acid salt and application thereof |
| JP2018531280A (en) * | 2015-08-25 | 2018-10-25 | ルジェニクス，インコーポレーテッド | Pharmaceutically acceptable salts of β-guanidinopropionic acid with improved properties and uses thereof |
| EP3340973A4 (en) * | 2015-08-25 | 2019-04-03 | Rgenix, Inc. | Pharmaceutically acceptable salts of -guanidinopropionic acid with improved properties and uses thereof |
| US10512623B2 (en) | 2015-08-25 | 2019-12-24 | Rgenix, Inc. | Pharmaceutically acceptable salts of B-Guanidinopropionic acid with improved properties and uses thereof |
| JP2021121597A (en) * | 2015-08-25 | 2021-08-26 | ルジェニクス，インコーポレーテッド | PHARMACEUTICALLY ACCEPTABLE SALTS OF β-GUANIDINOPROPIONIC ACID WITH IMPROVED PROPERTIES AND USES THEREOF |
| CN108472269B (en) * | 2015-08-25 | 2021-11-02 | 因思博纳公司 | Pharmaceutically acceptable beta-guanidinopropionates having improved properties and use thereof |
| CN114057611A (en) * | 2015-08-25 | 2022-02-18 | 因思博纳公司 | Pharmaceutically acceptable beta-guanidinopropionates having improved properties and use thereof |
| JP7134294B2 (en) | 2015-08-25 | 2022-09-09 | インスピルナ，インコーポレーテッド | Pharmaceutically acceptable salts of β-guanidinopropionic acid with improved properties and uses thereof |
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Application publication date: 20130102 |