Method for preparing 3-hydroxy butyrate

A technology of hydroxybutyrate and hydroxybutyrate, applied in the field of preparation of 3-hydroxybutyrate, can solve the problems of large production equipment requirements, high risk factor, long reaction time, etc. Simple and safe operation, the effect of short reaction time

Inactive Publication Date: 2019-05-24
宣城菁科生物科技有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing preparation method of 3-hydroxybutyrate often requires a pressurized reaction, which has a high risk factor. It is difficult to realize a reaction under normal pressure in the scale-up industrial production process, and the requirements for operators and production equipment are relatively large, and the reaction time is long.

Method used

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  • Method for preparing 3-hydroxy butyrate

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] A kind of preparation method of 3-hydroxybutyrate sodium that the present invention proposes, comprises the following steps:

[0021] S1. Add 0.93g of aluminum-nickel alloy catalyst accounting for 0.7% of its weight to 132.8g of 98% ethyl acetoacetate, carry out acyl hydrogenation reaction at normal pressure and 40°C, the reaction time is 10h, and suction filter after the reaction is completed , 129.5 g of ethyl 3-hydroxybutyrate was obtained, and the yield was 98.0%;

[0022] S2. Dissolve 129.5 g of ethyl 3-hydroxybutyrate in 388.5 g of water, the ratio of solid to liquid is 1:3, and then add 39.6 g of 99% sodium hydroxide, among which, ethyl 3-hydroxybutyrate and sodium hydroxide The molar ratio was 1:1, and reacted at 10°C for 2 hours. After the reaction, activated carbon was added to decolorize, filtered, and the filtrate was concentrated, crystallized, and dried to obtain 122.7 g of sodium 3-hydroxybutyrate with a yield of 98.5%.

[0023] The purity of the prepare...

Embodiment 2

[0025] A kind of preparation method of 3-hydroxybutyrate potassium that the present invention proposes, comprises the following steps:

[0026] S1. Add 1.06g of aluminum-nickel alloy catalyst accounting for 0.8% of its weight to 132.8g of 98% ethyl acetoacetate, carry out acyl hydrogenation reaction at normal pressure and 60°C, the reaction time is 12h, and suction filter after the reaction is completed , 130.44 g of ethyl 3-hydroxybutyrate was obtained, and the yield was 98.7%;

[0027] S2. Dissolve 130.44 g of ethyl 3-hydroxybutyrate in 456.5 g of water, the ratio of solid to liquid is 1:3.5, and then add 58 g of potassium hydroxide, wherein the molar ratio of 3-hydroxybutyrate to potassium hydroxide is 1:1.05, reacted at 10°C for 4 hours, after the reaction was completed, activated carbon was added for decolorization, filtered, the filtrate was concentrated, crystallized, and dried to obtain 140.35 g of potassium 3-hydroxybutyrate with a yield of 99.0%.

[0028] HPLC was u...

Embodiment 3

[0030] A kind of preparation method of 3-hydroxybutyrate calcium that the present invention proposes, comprises the following steps:

[0031] S1. Add 1.33g of aluminum-nickel alloy catalyst accounting for 1.0% of its weight to 132.8g of 98% ethyl acetoacetate, carry out acyl hydrogenation reaction at normal pressure and 80°C, the reaction time is 14h, and suction filter after the reaction is completed , 130.84 g of ethyl 3-hydroxybutyrate was obtained, and the yield was 99.0%;

[0032] S2. Dissolve 130.84g of ethyl 3-hydroxybutyrate in 523.4g of water, the ratio of solid to liquid is 1:4, and then add 40.3g of calcium hydroxide. Among them, the molar ratio of 3-hydroxybutyrate to calcium hydroxide 1:0.55, react at 15°C for 6h, after the reaction, add activated carbon to decolorize, filter, concentrate the filtrate, crystallize, dry to obtain 121.8g of calcium 3-hydroxybutyrate with a yield of 98.5%.

[0033] HPLC was used to detect the purity of the prepared calcium 3-hydroxy...

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Abstract

The invention discloses a method for preparing 3-hydroxy butyrate, and relates, and relates to the technical field of chemical synthesis and comprises the following steps of: adding an aluminum-nickelalloy catalyst into ethyl acetoacetate, carrying out acyl hydrogenation reaction at the temperature of 40-100 DEG C under a normal pressure, and carrying out suction filtration after the reaction isfinished to obtain 3- hydroxyl butyrate ethyl; dissolving the 3-hydroxybutyrate ethyl in water, adding inorganic base for reaction, decolorizing with activated carbon after reaction, filtering, concentrating the filtrate, crystallizing, and drying to obtain the 3-hydroxy butyrate. The method has the advantages of short reaction steps, cheap and easily obtained raw materials, mild reaction conditions, no need of pressurization, simple and safe operation and low requirement on production equipment; the adopted aluminum-nickel alloy catalyst is simply and easily obtained, can be recycled and reused, the production cost can be better controlled, the prepared product has high purity, the yield is high and the cost advantage is obvious, and the method is suitable for industrial production.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a preparation method of 3-hydroxybutyrate. Background technique [0002] 3-Hydroxybutyrate (3-HB) 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. The nature of 3-hydroxybutyric acid is unstable, it is easy to remove the hydroxyl group, and it is also easy to self-polymerize, so it is generally prepared as 3-hydroxybutyrate for preservation. The existing preparation method of 3-hydroxybutyrate often requires a pressurized reaction, which has a high risk factor. It is difficult to realize a reaction under normal pressure in the scale-up industrial production process, and the requirements for operators and production equipment are relatively large, and the reaction time is long. . Contents of the invention [0003] Based on t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/41C07C59/01
Inventor 李玉喜徐强徐海姜娜周慧萍
Owner 宣城菁科生物科技有限公司
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