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A betaine ester and butyl technology is applied in the production field of butyl betaine ester, and can solve the problems of increasing the synthesis cost and high selling price of γ-butyl betaine ester
Inactive Publication Date: 2009-09-23
潍坊祥维斯化学品有限公司
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Abstract
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Problems solved by technology
[0003] The synthesis of ethyl γ-bromobutyrate requires the use of bromine as a raw material,
Method used
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Examples
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Effect test
Embodiment 1
[0012] Example 1: 136.6g of methyl γ-chlorobutyrate (1.0mol, 99%), 89g of trimethylamine (1.5mol), and 180g of methanol were added to a 1L autoclave, sealed and stirred to raise the temperature to 85°C, and the reaction was kept for 10h. After the reaction was completed, the temperature was lowered to room temperature, and the material was discharged. Excess trimethylamine was distilled off, the temperature was lowered to 0-5°C to precipitate, and white crystals were obtained by filtration, which was washed with a small amount of acetone. The product was vacuum-dried at 60°C for 5 hours, the finished product was 166g, the HPLC content was 99.2%, and the yield was 85%.
Embodiment 2
[0013] Example 2: Add 150.6g of ethyl γ-chlorobutyrate (1.0mol, 99%), 89g of trimethylamine (1.5mol), and 180g of absolute ethanol into a 1L autoclave, stir and raise the temperature to 85°C after airtight, and keep the temperature for 10h . After the reaction was completed, the temperature was lowered to room temperature, and the material was discharged. Excess trimethylamine was distilled off, the temperature was lowered to 0-5°C to precipitate, and white crystals were obtained by filtration, which was washed with a small amount of acetone. The product was vacuum-dried at 70°C for 5 hours, the finished product was 191g, the HPLC content was 99.5%, and the yield was 91%.
Embodiment 3
[0014] Example 3: Add 136.6g gamma-chlorobutyric acid methyl ester (1.0mol, 99%), 118g trimethylamine (2.0mol, 99%), 180g methanol in a 1L autoclave, stir and heat up to 85°C after airtight, heat preservation reaction 10h. After the reaction was completed, the temperature was lowered to room temperature, and the material was discharged. Excess trimethylamine was distilled off, the temperature was lowered to 0-5°C to precipitate, and white crystals were obtained by filtration, which was washed with a small amount of acetone. The product was vacuum-dried at 60° C. for 5 hours to obtain 170 g of the finished product, the HPLC content was 99.3%, and the yield was 87%.
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Abstract
The invention discloses a method for preparing gamma-butyrobetaine ester, which uses gamma-chloro butyric ester and trimethylamine as raw materials and alcohol as a solvent. The raw materials and the solvent are heated to react in a high-pressure autoclave, and products of the gamma-butyrobetaine ester are obtained by concentrating processing and fine purification. The gamma-butyrobetaine ester is methyl ester or ethyl ester. The feeding mol ratio of the gamma- chloro butyric ester to the trimethylamine is 1:1.2-3.0, wherein the degree of purity of the gamma-chloro butyric ester is not less than 97 percent, and the degree of purity of the trimethylamine is more than 98 percent. The alcohol as the solvent is one of methanol, absolute ethyl alcohol, propanol, or isopropanol, and the use level of the alcohol is 1-5 times higher than that of the gamma-chloro butyric ester. The reaction is carried out at the temperature of 50-120 DEG C and the high pressure for 5-24h in an airtight mode. Because the technical scheme is adopted, the preparing cost is decreased, the domestic blank for preparing the gamma-butyrobetaine ester is replenished, and the mol yield of the products is enhanced and can reach more than 90 percent.
Description
technical field [0001] The invention relates to a production method of butyl betaine derivatives, in particular to a production method of butyl betaine ester. Background technique [0002] γ-Butyl betaine ester belongs to the derivatives of butyl betaine, and has many uses in the fields of medicine and hygiene, daily chemical and so on. The method of synthesizing γ-butyl betaine ester abroad is to pass ethyl γ-bromobutyrate into pure trimethylamine gas in acetone solvent, which takes about 3 hours, and the amount of trimethylamine is the mole number of γ-bromobutyrate 2 times, then sealed at room temperature overnight reaction, the yield of the product is about 85%. [0003] The synthesis of ethyl γ-bromobutyrate requires bromine as a raw material, so the price is relatively high, which virtually increases the synthesis cost of γ-butyl betaine ester. Contents of the invention [0004] The technical problem to be solved by the present invention is to provide a relatively ...
Claims
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Application Information
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