Method for preparing 3- hydroxybutyrate

A technology of hydroxybutyrate and hydroxybutyric acid, which is applied in the field of preparation of 3-hydroxybutyrate, can solve the problems of low purity and high cost of 3-hydroxybutyrate, so as to improve product yield, save material loss and Effects of energy consumption and production cost saving

Inactive Publication Date: 2019-02-22
SHANGHAI SHINE HIGH INT TRADE CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The problem solved by the present invention is that in the prior art, the disadvantages of high cost and low purity of preparing 3-hydroxybutyrate by chemical method

Method used

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  • Method for preparing 3- hydroxybutyrate

Examples

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no. 1 example

[0037] refer to figure 1 , the preparation method of the 3-hydroxybutyrate of the present embodiment, comprising:

[0038] (1) provide ethyl 3-hydroxybutyrate or methyl 3-hydroxybutyrate, and hydrolyze with a basic catalyst to obtain 3-hydroxybutyrate;

[0039] (2) 3-hydroxybutyric acid is reacted with an inorganic base to obtain 3-hydroxybutyrate.

[0040] In this embodiment, the basic catalyst is sodium hydroxide, potassium hydroxide, calcium hydroxide, magnesium hydroxide or lithium hydroxide, ethyl 3-hydroxybutyrate or methyl 3-hydroxybutyrate and alkali catalyst The molar ratio is 1:2.5~4.5. ,

[0041] In this embodiment, the molar ratio of the 3-hydroxybutyric acid to the inorganic base is 2 to 2.1:1.5, and the inorganic base is potassium hydroxide, calcium hydroxide, magnesium hydroxide or sodium hydroxide, corresponding to the obtained The 3-hydroxybutyrate is potassium 3-hydroxybutyrate, calcium 3-hydroxybutyrate, magnesium 3-hydroxybutyrate or sodium 3-hydroxybut...

no. 2 example

[0057] Add 200 grams of water into the reaction vessel, add 130 grams of ethyl 3-hydroxybutyrate or methyl 3-hydroxybutyrate under stirring to dissolve, after it is completely dissolved, add 166 grams of lithium hydroxide, and then heat up to 35°C for constant temperature reaction 24 hours.

[0058] After the reaction is completed, distill off water below 20°C, cool down to 0°C, add ethanol, fully stir and disperse for 2 hours, cool down to below 0°C to crystallize, keep warm at 0°C-5°C for 24 hours, and separate by suction filtration , washed the solid with ethanol, and dried at 35° C. to obtain 147 grams of 3-hydroxybutyric acid product, with a yield of 90.1%.

[0059] Take the finished product of 3-hydroxybutyric acid and put it into the reaction container, then add ethanol, stir to dissolve, add 105 grams of calcium hydroxide, and then raise the temperature to 45°C for 12 hours of constant temperature reaction. 0°C, add isopropanol to fully stir and disperse, cool down to...

no. 3 example

[0061] Add 300 grams of water into the reaction vessel, add 150 grams of ethyl 3-hydroxybutyrate or methyl 3-hydroxybutyrate under stirring to dissolve, after completely dissolving, add 156 grams of potassium hydroxide, and then raise the temperature to 45°C for constant temperature reaction 24 hours.

[0062] After the reaction is completed, distill off the water below 40°C, cool down to 0°C, add isopropanol, stir and disperse for 12 hours, cool down to below 0°C to crystallize, and keep warm at 0°C-5°C for 24 hours, pump After separation by filtration, the solid was washed with ethanol and dried at 55° C. to obtain 176 g of 3-hydroxybutyric acid with a yield of 95.1%.

[0063] Take the finished product of 3-hydroxybutyric acid and add it to the reaction container, then add isopropanol, stir to dissolve, add 125 grams of magnesium hydroxide, then raise the temperature to 55°C and react at a constant temperature for 12 hours. Alcohol, lower the temperature to 0°C, add ethanol...

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Abstract

The invention discloses a method for preparing 3-hydroxybutyrate. The method comprises the steps that (1) 3-ethyl hydroxybutyrate or 3-methyl hydroxybutyrate is provided and is hydrolyzed through a base catalyst to obtain 3-hydroxybutyric acid; and (2) the 3-hydroxybutyric acid reacts with an inorganic base to obtain the 3- hydroxybutyrate. Through the method, an aquatic salt forming mode is adopted, reacting is more complete, the reaction time is saved, energy consumption and material losses are lowered, the product yield is improved, and the production cost is saved. The concentration process in preparation of 3-hydroxybutyrate crude products is omitted, the series of processes of refining concentration of anhydrous ethanol, adding of acetone for crystallization, filtering, washing, drying and the like in preparing of 3-hydroxybutyrate finished products are omitted, an organic solvent, namely, acetone is omitted, material losses and energy consumption for the corresponding processesare reduced, and the production cost of the 3-hydroxybutyrate is greatly lowered. The heating process in roughing and refining of the 3-hydroxybutyrate is reduced, the problem that the 3-hydroxybutyrate finished products are easily affected with damp is also solved through the aquatic salt forming mode, and the quality of the 3-hydroxybutyrate is guaranteed.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a preparation method of 3-hydroxybutyrate. Background technique [0002] 3-Hydroxybutyric acid contains two functional groups, hydroxyl and carboxyl, and has the comprehensive properties of alcohol and carboxyl. It is an important pharmaceutical raw material and pharmacological reagent. Among them, (R)-3-hydroxybutyric acid is the isomer of R-configuration in the racemate of 3-hydroxybutyric acid, and it is an optically active chiral compound with a CAS number of 625-72-9 . (R)-3-Hydroxybutyric acid is a compound produced by the metabolism of long-chain fatty acids in the liver in mammals. It exists in plasma and peripheral tissues as the main ketone body, and has good penetration ability and Rapid diffusion ability, can be used as an energy source in most tissues of the body. Generally, R-3-HB exists in various salt forms. In addition to its nutritional function, (R)-3-hydro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/41C07C59/01
CPCC07C51/09C07C51/412C07C59/01B01J23/02C07C51/43B01J23/04C07C51/44
Inventor 呼延旺
Owner SHANGHAI SHINE HIGH INT TRADE CO LTD
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