CN101538214A - Method for preparing gamma-butyrobetaine and hydrochloride thereof - Google Patents
Method for preparing gamma-butyrobetaine and hydrochloride thereof Download PDFInfo
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- CN101538214A CN101538214A CN200910014909A CN200910014909A CN101538214A CN 101538214 A CN101538214 A CN 101538214A CN 200910014909 A CN200910014909 A CN 200910014909A CN 200910014909 A CN200910014909 A CN 200910014909A CN 101538214 A CN101538214 A CN 101538214A
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- butyrobetaine
- hydrochloride
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Abstract
The invention discloses a method for preparing gamma-butyrobetaine and hydrochloride thereof, which uses gamma-chloro butyric acid and trimethylamine as raw materials. On the premise that a catalytic agent is added, a reaction is carried out at the temperature of 60-120 DEG C and the pressure of 0.4-0.8MPa for 3-10h, or at the temperature of 30-35 DEG C and the ordinary pressure for 2 to 4 days to prepare the gamma-butyrobetaine. The catalytic agent is potassium halide or sodium halide, and the use level of the catalytic agent is 1 to 5 percent of the weight of the gamma-chloro butyric acid. After the reaction, finished products of the gamma-butyrobetaine are obtained by pressure reduction, concentration, filtration, washing and drying; or after hydrochloric acid is added to crude products of the gamma-butyrobetaine, products of gamma-butyrobetaine hydrochloride are obtained by concentration, filtration, washing and drying. Because the technical scheme is adopted, the domestic blank of the method for preparing the gamma-butyrobetaine and the hydrochloride thereof is replenished, and the invention is suitable for market demands and enriches the life of people.
Description
Technical field
The present invention relates to technical field of chemistry, relate in particular to the production method of chemical products.
Background technology
Gamma-butyrobetaine can prepare the L-carnitine by the B-hydroxylase catalysis synthesis process, and the L-carnitine more and more is subjected to people's attention as a kind of novel nutritive substance, at present domestic relevant gamma-butyrobetaine is synthetic almost not to be had, and therefore developing gamma-butyrobetaine has extensive market prospects.
Summary of the invention
Technical problem to be solved by this invention provides a kind of production gamma-butyrobetaine that fills the domestic gaps and the method for hydrochloride thereof.
For solving the problems of the technologies described above, technical scheme of the present invention is: producing the method for gamma-butyrobetaine, is to be raw material with γ-chloro butyric acid and Trimethylamine 99, and gamma-butyrobetaine is produced in reaction under the prerequisite that adds catalyzer.
Described reaction is under 60～120 ℃, preferred 90 ℃, and under 0.4～0.8MPa, reaction 3～10h, preferred 5～6h.
Described reaction is under 30～35 ℃, synthesis under normal pressure 2～4 days, preferred 3 days.
Described γ-chloro butyric acid purity 〉=95%, Trimethylamine 99 consumption are 2～8 times of γ-chloro butyric acid mole number, and preferred 3 times feed intake, and Trimethylamine 99 is the aqueous solution or pure product; Preferred Trimethylamine 99 is that mass content is 30% the aqueous solution.
Described catalyzer is potassium halide or sodium halide, and as potassiumiodide, sodium iodide, Potassium Bromide or Sodium Bromide, consumption is 1～5%, preferred 1% of γ-chloro butyric acid weight.
After reaction is finished, through known decompression, concentrate, filtration, washing and oven dry obtain the gamma-butyrobetaine finished product.
The method of producing the gamma-butyrobetaine hydrochloride is to produce gamma-butyrobetaine hydrochloride product add hydrochloric acid in gamma-butyrobetaine after, or after in the gamma-butyrobetaine crude product, adding hydrochloric acid, through known decompression, concentrate, filtration, washing and oven dry obtain the gamma-butyrobetaine hydrochloride.
Owing to adopted technique scheme, filled up the blank of domestic production gamma-butyrobetaine and hydrochloride method thereof, adapted to the demand in market, enriched people's life.
Embodiment
Below in conjunction with embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
In the 1L autoclave, add 123g γ-chloro butyric acid, 590g30% trimethylamine aqueous solution, potassiumiodide 1.23g, airtight back is stirred and is warming up to 90 ℃, under 0.4MPa, keep thermotonus 6h, cooling discharge removes excessive Trimethylamine 99 under reduced pressure, continuing to be concentrated into a large amount of white crystals occurs, filtering product is also with a small amount of 95% washing with alcohol, and oven dry obtains 100g gamma-butyrobetaine, yield 68.9%.
Embodiment 2
In three mouthfuls of reaction flasks of 1L, add 123g γ-chloro butyric acid, 590g30% trimethylamine aqueous solution, potassiumiodide 1.23g, stir down and keep 30-35 ℃, reaction 72h, remove excessive Trimethylamine 99 under reduced pressure, continuing to be concentrated into a large amount of white crystals occurs, filtering product is also with a small amount of 95% washing with alcohol, and oven dry obtains 89.3g gamma-butyrobetaine, yield 61.5%.
Embodiment 3
In the 1L autoclave, add 123g γ-chloro butyric acid, 590g30% trimethylamine aqueous solution, potassiumiodide 1.23g, airtight back is stirred and is warming up to 90 ℃, under 0.6MPa, keeps thermotonus 6h, reaction finishes and reduces to room temperature, discharging removes excessive Trimethylamine 99 under reduced pressure, adds the 100g concentrated hydrochloric acid under the room temperature, continuing to be concentrated into a large amount of white crystals occurs, filtering product is also with a small amount of 95% washing with alcohol, and oven dry obtains 136g gamma-butyrobetaine hydrochloride, yield 75%.
Embodiment 4
In the 1L autoclave, add 123g γ-chloro butyric acid, 590g30% trimethylamine aqueous solution, potassiumiodide 1.23g, airtight back is stirred and is warming up to 90 ℃, under 0.8MPa, reaction 5h, is γ-chloro butyric acid with ram pump with ratio: 30% Trimethylamine 99: the 2857g compound of catalyzer=123: 590: 1.23 at the uniform velocity adds in the autoclave with the speed of 143g/h, and is reinforced simultaneously from the speed discharging of discharge port with 143g/h.After all raw materials add, continue to lower the temperature behind the insulation reaction 5h, merge all reaction solutions and remove excessive Trimethylamine 99 under reduced pressure, the pH value of adjusting concentrated solution is neutral, at room temperature add the 500g concentrated hydrochloric acid, continue to be concentrated into a large amount of white crystals and occur, filtering product is also with a small amount of 95% washing with alcohol, dry 695g gamma-butyrobetaine hydrochloride, yield 76.5%.
Embodiment 5
In three mouthfuls of reaction flasks of 1L, add 123g γ-chloro butyric acid, 590g30% trimethylamine aqueous solution, potassiumiodide 1.23g, stir down and keep 30-35 ℃, reaction 72h, remove excessive Trimethylamine 99 under reduced pressure, add the 100g concentrated hydrochloric acid under the room temperature, continue to be concentrated into a large amount of white crystals and occur, filtering product is also with a small amount of 95% washing with alcohol, oven dry obtains 127.2g gamma-butyrobetaine hydrochloride, yield 70.0%.
Claims (7)
1. produce the method for gamma-butyrobetaine, it is characterized in that: present method is to be raw material with γ-chloro butyric acid and Trimethylamine 99, and the mode that adds catalyst reaction is produced gamma-butyrobetaine.
2. the method for production gamma-butyrobetaine as claimed in claim 1 is characterized in that: described reaction is under 60～120 ℃, under 0.4～0.8MPa, and reaction 3～10h.
3. the method for production gamma-butyrobetaine as claimed in claim 1 is characterized in that: described reaction is under 30～35 ℃, synthesis under normal pressure 2～4 days.
4. the method for production gamma-butyrobetaine as claimed in claim 1 is characterized in that: described Trimethylamine 99 consumption is 2～8 times of γ-chloro butyric acid mole number.
5. as the method for claim 1 or 4 described production gamma-butyrobetaines, it is characterized in that: described Trimethylamine 99 is the aqueous solution or pure product.
6. the method for production gamma-butyrobetaine as claimed in claim 1 is characterized in that: described catalyzer is potassium halide or sodium halide, and consumption is 1～5% of γ-chloro butyric acid weight.
7. produce the method for gamma-butyrobetaine hydrochloride, it is characterized in that: in the gamma-butyrobetaine of producing, add hydrochloric acid and produce gamma-butyrobetaine hydrochloride product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910014909A CN101538214A (en) | 2009-04-24 | 2009-04-24 | Method for preparing gamma-butyrobetaine and hydrochloride thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN200910014909A CN101538214A (en) | 2009-04-24 | 2009-04-24 | Method for preparing gamma-butyrobetaine and hydrochloride thereof |
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| CN101538214A true CN101538214A (en) | 2009-09-23 |
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| CN200910014909A Pending CN101538214A (en) | 2009-04-24 | 2009-04-24 | Method for preparing gamma-butyrobetaine and hydrochloride thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102666476A (en) * | 2009-10-22 | 2012-09-12 | 格林代克斯联合股份公司 | Use of 4-[ethyl(dimethyl)ammonio]butanoate in the treatment of cardiovascular disease |
| CN102807499A (en) * | 2012-08-27 | 2012-12-05 | 陈林世 | Method for preparing betaine hydrochloride |
| RU2720985C1 (en) * | 2019-07-04 | 2020-05-15 | Федеральное государственное унитарное предприятие "Научно-исследовательский институт гигиены, профпатологии и экологии человека" Федерального медико-биологического агентства | Method of producing gamma-butirobethaine and hydrochloride thereof |
-
2009
- 2009-04-24 CN CN200910014909A patent/CN101538214A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102666476A (en) * | 2009-10-22 | 2012-09-12 | 格林代克斯联合股份公司 | Use of 4-[ethyl(dimethyl)ammonio]butanoate in the treatment of cardiovascular disease |
| CN102666476B (en) * | 2009-10-22 | 2014-07-09 | 格林代克斯联合股份公司 | Use of 4-[ethyl(dimethyl)ammonio]butanoate in the treatment of cardiovascular disease |
| CN102807499A (en) * | 2012-08-27 | 2012-12-05 | 陈林世 | Method for preparing betaine hydrochloride |
| RU2720985C1 (en) * | 2019-07-04 | 2020-05-15 | Федеральное государственное унитарное предприятие "Научно-исследовательский институт гигиены, профпатологии и экологии человека" Федерального медико-биологического агентства | Method of producing gamma-butirobethaine and hydrochloride thereof |
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Application publication date: 20090923 |