CN102838502A - Preparation method of L-phenylalanine nitrate - Google Patents
Preparation method of L-phenylalanine nitrate Download PDFInfo
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- CN102838502A CN102838502A CN 201110172738 CN201110172738A CN102838502A CN 102838502 A CN102838502 A CN 102838502A CN 201110172738 CN201110172738 CN 201110172738 CN 201110172738 A CN201110172738 A CN 201110172738A CN 102838502 A CN102838502 A CN 102838502A
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- phenylalanine
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Abstract
The invention discloses a preparation method of L-phenylalanine nitrate, which comprises the steps of uniformly stirring L-phenylalanine with water, dropwise adding nitric acid at a concentration of 65% within 30 minutes at 20 DEG C to 60 DEG C, and continuing to keep warm and stir for 20 minutes, heating to 50-65 DEG C, conducting vacuum dewatering, cooling dewatered feed liquid to be less than or equal to 10 DEG C to separate out L- phenylalanine nitrate solid and conducting filtration and drying to obtain a finished product of the L- phenylalanine nitrate. The prepared L-phenylalanine nitrate product has few impurities and good quality. The purity is greater than 99% without recrystallization; the product quality is ensured; the working procedure and the production time are saved; and the production efficiency is improved. According to the preparation method of the L-phenylalanine nitrate, mother liquor is recycled, so that the yield is increased, and the cost is lowered. Valuable water sources are saved; no byproducts are generated in the production, and almost no waste gas, waste water or industrial residue is produced. The preparation method of the L-phenylalanine nitrate is reasonable, simple and environment-friendly in process and suitable for industrial production.
Description
Technical field
The present invention relates to a kind of preparation method of amidates, particularly a kind of preparation method of L-phenylalanine(Phe) nitrate salt.
Background technology
Amino acid is the base substance that constitutes the Animal nutrition desired protein.General people self generate or can obtain to satisfy through food each seed amino acid of somagenic need.But under special situation as human infantile period; Under the situation that sick, injured or large amount of exercise is taken exercise, for growth needs, recover various metabolic balances in the body, strengthening immunity and sportsmen regain one's strength as early as possible; Increase muscle strength, just need extra each seed amino acid that replenishes.
L-phenylalanine(Phe) chemical name becomes: L-2-amino-3-phenylpropionic acid.The L-phenylalanine(Phe) is one of essential amino acid, has the die aromatischen Aminosaeuren of physiologically active.Be that human body and animal can not lean on one of own nature synthetic indispensable amino acid, be the important composition of built amino-acid transfusion; Being used for medical aspect, is the midbody of amino acids cancer therapy drugs such as phenylpropyl alcohol ammonia benzyl, formic acid Sarkolizin, also is to produce suprarenin, thyroxine and melanic raw material; Existing research shows that the carrier that the L-phenylalanine(Phe) can be used as cancer therapy drug directly imports cancer knurl district with drug molecule, and its effect is other amino acid whose 3～5 times.So both can suppress the growth of cancer knurl, can reduce the toxic side effect of medicine again.
Because amino acid salts analogy amino acid is dissolved in the water easily; It is transformed into amino acid through effects such as oxydase in vivo at last; Compare and directly take amino acid more easily by the health absorption, take so amino acid is all made amidates usually, it is more generally to make amino acid whose hydrochloride.The U.S. parties concerned discover that amino acid whose nitrate salt more helps amino acid and absorbed by health recently, therefore the L-phenylalanine(Phe) are made into L-phenylalanine(Phe) nitrate salt and take, and will change into the L-phenylalanine(Phe) more easily and absorbed by health.Dosage can be littler when it used, and oral absorption efficient can be higher.
Summary of the invention
The present invention is in order to obtain being provided by the L-phenylalanine(Phe) nitrate salt of health absorption more easily a kind of preparation method of L-phenylalanine(Phe) nitrate salt.
The technical scheme that the present invention takes for the technical problem that exists in the above-mentioned technology of solution is:
The preparation method of a kind of L-phenylalanine(Phe) nitrate salt of the present invention is following: L-phenylalanine(Phe) and water are stirred, and dropping concentration is 65% nitric acid, and controlled temperature is at 20 ℃～60 ℃; Dropwise in 30 minutes; Continuing insulated and stirred 20 minutes, and be warming up to 50 ℃～65 ℃ vaccum dewaterings then, dewatered feed liquid is cooled to≤and 10 ℃; Separate out solid, through filtration, the dry L-phenylalanine(Phe) nitrate salt finished product that gets.Liquid after the filtration recycles as mother liquor aborning.
The mol ratio of above-mentioned L-phenylalanine(Phe) and nitric acid is 1: 1～1.1.
The ratio of above-mentioned L-phenylalanine(Phe) and water is 1g: 2ml.
Advantage and positively effect that the present invention has are: the raw material that the present invention adopts is the L-phenylalanine(Phe) of food grade and the nitric acid of chemical reagent-grade, so the L-phenylalanine(Phe) nitrate salt product impurity of producing is few, quality is good.Just reach more than 99% without recrystallization purity, both guaranteed quality, saved operation and PT again, improved production efficiency.The present invention utilizes Recycling Mother Solution to use, and has improved yield, has reduced cost.Practiced thrift precious water resource.The present invention simultaneously is no coupling product aborning, produces the three wastes hardly.Preparing method's technology of the present invention is reasonable, simple, environmental protection, is fit to industrialized production.
Embodiment
The solubleness of L-phenylalanine(Phe) in water is less among the present invention, need add a certain amount of water during reaction, and water is deionized purified water, to guarantee the quality of product.Below just directly call in the narration and be water.
The mol ratio of L-phenylalanine(Phe) and nitric acid should be 1: 1 among the present invention, but for the L-phenylalanine(Phe) is reacted completely, nitric acid dosage should be more bigger than L-phenylalanine(Phe).Scope is between 1～1.1 mole.
Temperature of reaction of the present invention should be controlled at below 60 ℃, and the vaccum dewatering temperature should be controlled at below 65 ℃.Otherwise can exert an adverse impact to product.
Liquid after the present invention will filter replaces water to recycle aborning as mother liquor; Owing to filter out in the liquid after the crystallization and do not have crystalline L-phenylalanine(Phe) nitrate salt in addition; So when it is used for next step production; The crystallization that is produced can both be separated out more than 95%, has improved actual recovery greatly.
For further understanding summary of the invention of the present invention, characteristics and effect, the following examples of giving an example now:
Embodiment 1
Take by weighing L-phenylpropionic acid 16.5g (0.1 mole) and put into reaction flask, add water 33ml, stir.While stirring the nitric acid 10g (0.1 mole) that drips 65% concentration, control reaction temperature dropwised at 55 ℃ in 20 minutes, and feed liquid is clarified gradually, continued to keep temperature to stir 20 minutes.Be warming up to 63 ℃ of vaccum dewaterings subsequently.Feed liquid after dewatering is cooled to 5 ℃, separates out the solid of white L-phenylalanine(Phe) nitrate salt, filtration, the dry L-phenylalanine(Phe) nitrate salt finished product that gets.Liquid after the filtration recycles as mother liquor aborning.
Embodiment 2
Take by weighing L-phenylpropionic acid 16.5g (0.1 mole) and put into reaction flask, add masterbatch 33ml, stir.While stirring the nitric acid 10g (0.1 mole) that drips 65% concentration, control reaction temperature dropwised at 40 ℃ in 10 minutes, and feed liquid is clarified gradually, continued to keep temperature to stir 20 minutes.Be warming up to 57 ℃ subsequently, vaccum dewatering.Feed liquid after dewatering is cooled to 10 ℃, separates out the solid of white L-phenylalanine(Phe) nitrate salt, filtration, the dry L-phenylalanine(Phe) nitrate salt finished product that gets.Liquid after the filtration recycles as mother liquor aborning.
Embodiment 3
Take by weighing L-phenylpropionic acid 16.5g (0.1 mole) and put into reaction flask, add masterbatch 33ml, stir.While stirring the nitric acid 10g (0.1 mole) that drips 65% concentration, control reaction temperature dropwised at 25 ℃ in 30 minutes, and feed liquid is clarified gradually, continued to keep temperature to stir 20 minutes.Be warming up to 50 ℃ subsequently, vaccum dewatering.Feed liquid after dewatering is cooled to 0 ℃, separates out the solid of white L-phenylalanine(Phe) nitrate salt, filtration, the dry L-phenylalanine(Phe) nitrate salt finished product that gets.Liquid after the filtration recycles as mother liquor aborning.
Claims (3)
1. the preparation method of a L-phenylalanine(Phe) nitrate salt is characterized in that the preparation method is following: under the room temperature L-phenylalanine(Phe) and water are stirred, drip concentration and be 65% nitric acid; Temperature is controlled at 20 ℃～60 ℃; Dropwise in 30 minutes, continued insulated and stirred 20 minutes, be warming up to then at 50 ℃～65 ℃ vaccum dewaterings; Dewatered feed liquid is cooled to≤and 10 ℃; Separate out solid, through filtration, the dry L-phenylalanine(Phe) nitrate salt finished product that gets, the liquid after the filtration recycles as mother liquor aborning.
2. the preparation method of L-phenylalanine(Phe) nitrate salt according to claim 1, the mol ratio that it is characterized in that L-phenylalanine(Phe) and nitric acid is 1: 1～1.1.
3. the preparation method of L-phenylalanine(Phe) nitrate salt according to claim 1, the ratio that it is characterized in that L-phenylalanine(Phe) and water is 1g: 2ml.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110172738 CN102838502A (en) | 2011-06-24 | 2011-06-24 | Preparation method of L-phenylalanine nitrate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110172738 CN102838502A (en) | 2011-06-24 | 2011-06-24 | Preparation method of L-phenylalanine nitrate |
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| CN102838502A true CN102838502A (en) | 2012-12-26 |
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| CN 201110172738 Pending CN102838502A (en) | 2011-06-24 | 2011-06-24 | Preparation method of L-phenylalanine nitrate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103664705A (en) * | 2013-12-13 | 2014-03-26 | 天津天成制药有限公司 | Citrulline nitrate synthesizing method |
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2011
- 2011-06-24 CN CN 201110172738 patent/CN102838502A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103664705A (en) * | 2013-12-13 | 2014-03-26 | 天津天成制药有限公司 | Citrulline nitrate synthesizing method |
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Application publication date: 20121226 |