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Method for synthesizing beta-hydroxymethyl butyrate

A technology of methyl hydroxybutyrate and methyl formate, which is applied in the field of synthesis of methyl β-hydroxybutyrate, can solve the problems of difficult storage and use of catalysts, and achieve cheap raw materials and catalysts, small scale, and mild reaction conditions Effect

Inactive Publication Date: 2013-01-09
DALIAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But the biggest disadvantage of this conventional carbonylation reaction method is that the reaction should be completed under high pressure (≥6.0MPa), and the catalyst is not easy to preserve and use. In addition, it is necessary to use toxic CO gas, so that this method can be used on a small scale. The application of fine products is subject to certain restrictions

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  • Method for synthesizing beta-hydroxymethyl butyrate
  • Method for synthesizing beta-hydroxymethyl butyrate
  • Method for synthesizing beta-hydroxymethyl butyrate

Examples

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example 1

[0030] Propylene oxide (analytically pure) was mixed with methanol to prepare a methanol solution with a concentration of 250mmol / L. Mix the catalyst cobalt acetate, cadmium iodide and methanol to prepare a methanol solution with a concentration of 8mmol / L, wherein the total concentration of cobalt acetate and cadmium iodide is 8mmol / L, and the molar ratio of cobalt acetate and cadmium iodide is 1:9 . The above methanol solution of the catalyst was mixed with the above methanol solution of propylene oxide. Add sodium acetate in the above mixed solution, its concentration in the mixed solution is 300mmol / L. A 100W high-pressure mercury lamp is placed inside a quartz photoreactor with a hollow interlayer, and circulating water is passed into the interlayer, and the entire reactor is placed in a water tank filled with water to cool the light source. Add 4ml of methanol solution containing 250mmol / L propylene oxide, 8mmol / L catalyst cobalt acetate and cadmium iodide, and 300mmol...

example 2

[0032] Propylene oxide (analytical pure) was mixed with methanol to prepare a methanol solution with a concentration of 1000mmol / L. Mix the catalyst cobalt acetate, cadmium iodide and methanol to prepare a methanol solution with a concentration of 16mmol / L, wherein the total concentration of cobalt acetate and cadmium iodide is 16mmol / L, and the molar ratio of cobalt acetate and cadmium iodide is 1:9 . The above methanol solution of the catalyst was mixed with the above methanol solution of propylene oxide. Add sodium acetate to the above mixed solution, and its concentration in the mixed solution is 900mmol / L. A 400W high-pressure mercury lamp is placed inside a quartz photoreactor with a hollow interlayer, and circulating water is passed into the interlayer, and the entire reactor is placed in a water tank filled with water to cool the light source. Add 4ml of methanol solution containing 1000mmol / L propylene oxide, 16mmol / L catalyst cobalt acetate and cadmium iodide, and ...

example 3

[0034] Propylene oxide (analytically pure) was mixed with methanol to prepare a methanol solution with a concentration of 250mmol / L. Mix the catalyst cobalt acetate, cadmium iodide and methanol to prepare a methanol solution with a concentration of 12mmol / L, wherein the total concentration of cobalt acetate and cadmium iodide is 12mmol / L, and the molar ratio of cobalt acetate and cadmium iodide is 1:9 . The above methanol solution of the catalyst was mixed with the above methanol solution of propylene oxide. Add sodium acetate to the above mixed solution, and its concentration in the mixed solution is 900mmol / L. A 400W high-pressure mercury lamp is placed inside a quartz photoreactor with a hollow interlayer, and circulating water is passed into the interlayer, and the entire reactor is placed in a water tank filled with water to cool the light source. Add 4ml of methanol solution containing 250mmol / L propylene oxide, 12mmol / L catalyst cobalt acetate and cadmium iodide, and ...

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Abstract

The invention discloses a method for synthesizing beta-hydroxymethyl butyrate, which mainly comprises the step of adding methyl formate with a concentration of between 125 and 625mmol / lL into a methanol solution containing propylene oxide with a concentration of between 250 and 1,000mmol / lL and a cobalt acetate and cadmium iodide catalyst with a concentration of between 8 and 16mmol / lL, wherein the molar ratio of cobalt acetate to cadmium iodide is 1: 9, a high-voltage mercury lamp with the power of between 100 and 400W is used to irradiate a reaction liquid for 15 to 55 hours, and the reaction temperature is between 25 and 60 DEG C. Preferably, sodium acetate with a concentration of between 300 and 900mmol / lL is also added into the methanol solution containing the propylene oxide with the concentration of between 250 and 1,000mmol / lL and the catalyst with the concentration of between 8 and 16mmol / lL. The method ensures that a carbonylation reaction gets simple and easy and has safe operation; and a non-precious metal compound adopted as the catalyst is easy to obtain and is also convenient to store and use. The product has low cost, and is suitable for the synthesis of the beta-hydroxymethyl butyrate with small scale and high added value.

Description

technical field [0001] The invention relates to a method for synthesizing methyl β-hydroxybutyrate. Background technique [0002] In recent years, as the demand for β-hydroxy acid esters in materials, medicine and industry has gradually increased, people's research on them has also been continuously strengthened. The traditional synthesis of β-hydroxy acid esters is the Reformatsky reaction. The reaction substrate of this method is α-halogenated ester, which is a commercial compound that is not easy to obtain, and a large amount of Zn powder is required in the reaction, and the yield of β-hydroxy acid ester is low, forcing people to find other methods to synthesize β - Hydroxy esters. So someone invented the carbonylation reaction of propylene oxide, carbon monoxide and methanol to synthesize methyl β-hydroxybutyrate, which is based on Co 2 (CO) 8 As a catalyst, it was reacted at 24.5MPa and 130°C for 4 hours. Although this method is better than the above-mentioned trad...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/675C07C67/343B01J31/04
Inventor 尹静梅徐波贾颖萍崔颖娜周广运高大彬
Owner DALIAN UNIV
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