CN106748870A - A kind of method for producing Acetyl Tyrosine - Google Patents
A kind of method for producing Acetyl Tyrosine Download PDFInfo
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- CN106748870A CN106748870A CN201510803570.9A CN201510803570A CN106748870A CN 106748870 A CN106748870 A CN 106748870A CN 201510803570 A CN201510803570 A CN 201510803570A CN 106748870 A CN106748870 A CN 106748870A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/02—Preparation of carboxylic acid amides from carboxylic acids or from esters, anhydrides, or halides thereof by reaction with ammonia or amines
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/22—Separation; Purification; Stabilisation; Use of additives
- C07C231/24—Separation; Purification
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of method for producing Acetyl Tyrosine, the method belongs to amino acids production field；The raw material that the production method is used includes：Tyrosine, chloroacetic chloride, deionized water, liquid caustic soda, hydrochloric acid, activated carbon, by operations such as acylation reaction, crystallisation by cooling, filtering, drying, crushing, packagings come finished product；The method is produced using common apparatus, has the advantages that simple production process, easy to operate, reaction condition be gentle, pollution-free waste discharge, and product Acetyl Tyrosine is important fine organic chemical industry's intermediate.
Description
Technical field：
The invention belongs to amino acids production field, more particularly to a kind of method for producing Acetyl Tyrosine.
Background technology：
Tyrosine is one kind of amino acid, and finished product is white crystalline body or crystalline powder, belongs to human body nonessential amino acid；Tyrosine is the considerable composition of the body constitutive protein matter of people, and tyrosine is contained in many dairy products, meat, fish, wheat, oat and the protein food comprising tyrosine, and tyrosine is widely used, can be used for medicine, biochemical reagents, food additives.Tyrosine acetylation is just directly obtained into Acetyl Tyrosine, so-called acetylation is exactly that, by the process on acetyl grouptransfer to amino acid side groups in amino acid, conventional acetylizing agent has chloroacetic chloride, aceticanhydride and glacial acetic acid etc.；Acetyl Tyrosine outward appearance is white crystals or crystalline powder, is important fine organic chemical industry's intermediate, is widely used in the fields such as medicine, agricultural chemicals, chemical industry.
The product is produced with tyrosine, chloroacetic chloride, deionized water, liquid caustic soda, hydrochloric acid, activated carbon as raw material.
The content of the invention：
Present invention mainly solves problem be to provide a kind of method for producing Acetyl Tyrosine, the method produces Acetyl Tyrosine with chemical reaction kettle, crystallization kettle, plate filter, dryer, pulverizer, packing machine as equipment with tyrosine, chloroacetic chloride, deionized water, liquid caustic soda, hydrochloric acid, activated carbon as raw material.
The technical solution adopted by the present invention is：
（1）By deionized water, liquid caustic soda, tyrosine, chloroacetic chloride by weight deionized water, liquid caustic soda, tyrosine, chloroacetic chloride=6.0-7.0:1:1.0:The ratio of 1.0-2.0 is sequentially sent to chemical reaction kettle, and vacuum is evacuated to after chemical reaction kettle is sealed, and while stirring gradually rises to 55-59 DEG C chemical reaction temperature in the kettle; stirring reaction 2.0-2.2 hours; after terminating the abundant acetylation of tyrosine, reaction, reaction solution is sent into crystallization kettle.
（2）The hydrochloric acid that concentration is 30% is sent into crystallization kettle, the pH value for adjusting reaction solution stops plus hydrochloric acid when being 4.3-4.35, at this moment the temperature of adjustment crystallization kettle is below 5 DEG C, crystallized after standing 24 hours and finished, all materials feeding filter in crystallization kettle is filtered off into liquid, liquid portion discharge is reclaimed, and remaining filter cake is Acetyl Tyrosine crude product.
（3）Acetyl Tyrosine crude product is sent into chemical reaction kettle, add warming while stirring after the deionized water of 5-6 times of filter cake weight, the activated carbon of 0.2-0.22 times of filter cake weight is added simultaneously, stirring decolouring terminates to decolourize after 1-1.2 hours, obtain destainer, destainer is sent into crystallization kettle, constant temperature keeps crystallizing for 24 hours below 5 DEG C, whole materials feeding filter filtering after crystallization, filtrate discharge is reclaimed, dried in solid portion feeding dryer, drying temperature is 42 DEG C -45 DEG C, drying time is 3.5-3.8 hours, then the material feeding pulverizer after drying is crushed, then the pulvis after crushing is sent into packing machine, packaging gets product.
Further technical scheme of the invention is：
Described chemical reaction kettle is 3 tonnes, ceramic liner.
Described filter is flame filter press.
The beneficial effects of the invention are as follows：There is provided a kind of method for producing Acetyl Tyrosine, the method uses common apparatus, has the advantages that process is simple, easy to operate, reaction condition be gentle, pollution-free waste discharge, and product Acetyl Tyrosine is important fine organic chemical industry's intermediate.
Specific embodiment
Embodiment 1：
By deionized water, liquid caustic soda, tyrosine, chloroacetic chloride by weight deionized water, liquid caustic soda, tyrosine, chloroacetic chloride=6.0:1:1.0:2.0 ratio is sequentially sent to chemical reaction kettle, and vacuum is evacuated to after chemical reaction kettle is sealed, and while stirring gradually rises to 55 DEG C chemical reaction temperature in the kettle; stirring reaction 2.2 hours; after terminating the abundant acetylation of tyrosine, reaction, reaction solution is sent into crystallization kettle.The hydrochloric acid that concentration is 30% is sent into crystallization kettle, the pH value for adjusting reaction solution stops plus hydrochloric acid when being 4.3, at this moment the temperature of adjustment crystallization kettle is below 5 DEG C, crystallized after standing 24 hours and finished, all materials feeding filter in crystallization kettle is filtered off into liquid, liquid portion discharge is reclaimed, and remaining filter cake is Acetyl Tyrosine crude product.Acetyl Tyrosine crude product is sent into chemical reaction kettle, add warming while stirring after the deionized water of 5 times of filter cake weight, the activated carbon of 0.2 times of filter cake weight is added simultaneously, stirring terminates to decolourize after decolourizing 1 hour, obtain destainer, destainer is sent into crystallization kettle, constant temperature keeps crystallizing for 24 hours below 5 DEG C, whole materials feeding filter filtering after crystallization, filtrate discharge is reclaimed, dried in solid portion feeding dryer, drying temperature is 42 DEG C, drying time is 3.8 hours, then the material feeding pulverizer after drying is crushed, then the pulvis after crushing is sent into packing machine, packaging gets product.
Embodiment 2：
By deionized water, liquid caustic soda, tyrosine, chloroacetic chloride by weight deionized water, liquid caustic soda, tyrosine, chloroacetic chloride=6.5:1:1.0:1.5 ratio is sequentially sent to chemical reaction kettle, and vacuum is evacuated to after chemical reaction kettle is sealed, and while stirring gradually rises to 57 DEG C chemical reaction temperature in the kettle; stirring reaction 2.1 hours; after terminating the abundant acetylation of tyrosine, reaction, reaction solution is sent into crystallization kettle.The hydrochloric acid that concentration is 30% is sent into crystallization kettle, the pH value for adjusting reaction solution stops plus hydrochloric acid when being 4.30, at this moment the temperature of adjustment crystallization kettle is below 5 DEG C, crystallized after standing 24 hours and finished, all materials feeding filter in crystallization kettle is filtered off into liquid, liquid portion discharge is reclaimed, and remaining filter cake is Acetyl Tyrosine crude product.Acetyl Tyrosine crude product is sent into chemical reaction kettle, add warming while stirring after the deionized water of 5.5 times of filter cake weight, the activated carbon of 0.21 times of filter cake weight is added simultaneously, stirring terminates to decolourize after decolourizing 1.1 hours, obtain destainer, destainer is sent into crystallization kettle, constant temperature keeps crystallizing for 24 hours below 5 DEG C, whole materials feeding filter filtering after crystallization, filtrate discharge is reclaimed, dried in solid portion feeding dryer, drying temperature is 43.5 DEG C, drying time is 3.65 hours, then the material feeding pulverizer after drying is crushed, then the pulvis after crushing is sent into packing machine, packaging gets product.
Embodiment 3：
By deionized water, liquid caustic soda, tyrosine, chloroacetic chloride by weight deionized water, liquid caustic soda, tyrosine, chloroacetic chloride=7:1:1.0:The ratio of 1.0-1.0 is sequentially sent to chemical reaction kettle, and vacuum is evacuated to after chemical reaction kettle is sealed, and while stirring gradually rises to 59 DEG C chemical reaction temperature in the kettle; stirring reaction 2.0 hours; after terminating the abundant acetylation of tyrosine, reaction, reaction solution is sent into crystallization kettle.The hydrochloric acid that concentration is 30% is sent into crystallization kettle, the pH value for adjusting reaction solution stops plus hydrochloric acid when being 4.35, at this moment the temperature of adjustment crystallization kettle is below 5 DEG C, crystallized after standing 24 hours and finished, all materials feeding filter in crystallization kettle is filtered off into liquid, liquid portion discharge is reclaimed, and remaining filter cake is Acetyl Tyrosine crude product.Acetyl Tyrosine crude product is sent into chemical reaction kettle, add warming while stirring after the deionized water of 6 times of filter cake weight, the activated carbon of 0.22 times of filter cake weight is added simultaneously, stirring terminates to decolourize after decolourizing 1 hour, obtain destainer, destainer is sent into crystallization kettle, constant temperature keeps crystallizing for 24 hours below 5 DEG C, whole materials feeding filter filtering after crystallization, filtrate discharge is reclaimed, dried in solid portion feeding dryer, drying temperature is 45 DEG C, drying time is 3.5 hours, then the material feeding pulverizer after drying is crushed, then the pulvis after crushing is sent into packing machine, packaging gets product.
Certainly, the present invention also has other implementation methods, and the improvement of any technology, principle and the technique done under without departing from spiritual background of the invention is within the scope of the present invention.
Claims (3)
1. a kind of method for producing Acetyl Tyrosine, the raw material for using includes：Tyrosine, chloroacetic chloride, deionized water, liquid caustic soda, hydrochloric acid, activated carbon, by operations such as acylation reaction, crystallisation by cooling, filtering, drying, crushing, packagings come finished product, it is characterised in that：
（1）By deionized water, liquid caustic soda, tyrosine, chloroacetic chloride by weight deionized water, liquid caustic soda, tyrosine, chloroacetic chloride=6.0-7.0:1:1.0:The ratio of 1.0-2.0 is sequentially sent to chemical reaction kettle, and vacuum is evacuated to after chemical reaction kettle is sealed, and while stirring gradually rises to 55-59 DEG C chemical reaction temperature in the kettle; stirring reaction 2.0-2.2 hours; after terminating the abundant acetylation of tyrosine, reaction, reaction solution is sent into crystallization kettle；
（2）The hydrochloric acid that concentration is 30% is sent into crystallization kettle, the pH value for adjusting reaction solution stops plus hydrochloric acid when being 4.3-4.35, at this moment the temperature of adjustment crystallization kettle is below 5 DEG C, crystallized after standing 24 hours and finished, all materials feeding filter in crystallization kettle is filtered off into liquid, liquid portion discharge is reclaimed, and remaining filter cake is Acetyl Tyrosine crude product；
（3）Acetyl Tyrosine crude product is sent into chemical reaction kettle, add warming while stirring after the deionized water of 5-6 times of filter cake weight, the activated carbon of 0.2-0.22 times of filter cake weight is added simultaneously, stirring decolouring terminates to decolourize after 1-1.2 hours, obtain destainer, destainer is sent into crystallization kettle, constant temperature keeps crystallizing for 24 hours below 5 DEG C, whole materials feeding filter filtering after crystallization, filtrate discharge is reclaimed, dried in solid portion feeding dryer, drying temperature is 42 DEG C -45 DEG C, drying time is 3.5-3.8 hours, then the material feeding pulverizer after drying is crushed, then the pulvis after crushing is sent into packing machine, packaging gets product.
2. a kind of method for producing Acetyl Tyrosine as claimed in claim 1, it is characterised in that：Described chemical reaction kettle is 3 tonnes, ceramic liner.
3. a kind of method for producing Acetyl Tyrosine as claimed in claim 1, it is characterised in that：Described filter is flame filter press.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510803570.9A CN106748870A (en) | 2015-11-20 | 2015-11-20 | A kind of method for producing Acetyl Tyrosine |
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| CN201510803570.9A CN106748870A (en) | 2015-11-20 | 2015-11-20 | A kind of method for producing Acetyl Tyrosine |
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| CN106748870A true CN106748870A (en) | 2017-05-31 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111153829A (en) * | 2019-12-26 | 2020-05-15 | 烟台鲁银药业有限公司 | Preparation method of N-acetyl-L-tyrosine |
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- 2015-11-20 CN CN201510803570.9A patent/CN106748870A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111153829A (en) * | 2019-12-26 | 2020-05-15 | 烟台鲁银药业有限公司 | Preparation method of N-acetyl-L-tyrosine |
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Application publication date: 20170531 |
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