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A kind of synthetic method of methyl hydroxytrimethyl acetate

A technology of methyl hydroxytrimethyl acetate and a synthesis method, which is applied in the field of synthesis of methyl hydroxytrimethyl acetate, can solve the problems of difficult catalyst recovery and treatment, unsuitable for industrial production, unfavorable economic benefits and the like, and achieves high industrial popularization. Prospects, improving the overall yield of the reaction, and the effect of high economic benefits

Active Publication Date: 2018-03-09
ITIC MEDCHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The above-mentioned methods have their own advantages and disadvantages: the first one is relatively simple, but due to the utilization of the disproportionation reaction, the highest product yield is no more than 50%, which is not suitable for industrialized production; the second method has a high yield, and can even reach 100%, but The oxidation reaction is carried out in a very fine aqueous solution, so it is difficult to deal with a large amount of water, and sodium 2,2-dimethyl-3-hydroxypropionate is easy to agglomerate in the reaction kettle, and subsequent treatment causes great difficulties
The third method also has problems such as post-processing difficulties
This document is the closest prior art of the present invention, and this method reaction condition is gentle, and yield is higher, but in the synthetic 2,2-dimethyl-3-hydroxypropanal reaction process, adding sodium carbonate is catalyst, and catalyst reclaims It is difficult to handle; during the synthesis of methyl hydroxytrimethyl acetate, sodium hydroxide reacts with chlorine gas, 2NaOH+CI 2 =NaCl+NaCIO+H 2 O, the sodium chloride needs to be filtered out at the end of the reaction, the follow-up operation is complicated and causes waste of raw materials, the yield is low, and it is not conducive to the improvement of economic benefits

Method used

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  • A kind of synthetic method of methyl hydroxytrimethyl acetate
  • A kind of synthetic method of methyl hydroxytrimethyl acetate
  • A kind of synthetic method of methyl hydroxytrimethyl acetate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] A synthetic method for methyl hydroxytrimethyl acetate, comprising the following steps:

[0050] The first step: aldol condensation reaction:

[0051] In a 500mL container, put 36.05g of isobutyraldehyde, 41.29g of formaldehyde solution with a mass concentration of 40%, and 0.7g of catalyst, and stir and react at a temperature of 60°C for 3h;

[0052] After the reaction was completed, the catalyst was removed by hot filtration, and the organic layer was separated by layers at room temperature;

[0053] The second step: oxidation and esterification reaction:

[0054] Put the organic layer separated in the first step above into a 500mL container, add 100mL of methanol, add 30mL of sodium hydroxide solution with a mass concentration of 40% at a temperature of 35°C, feed oxygen until the pressure is 0.5Mpa, and stir for 1h , Remove formaldehyde and water to obtain methyl hydroxytrimethylacetate.

Embodiment 2

[0056] A synthetic method for methyl hydroxytrimethyl acetate, comprising the following steps:

[0057] The first step: aldol condensation reaction:

[0058] In a 500mL container, put 36.05g of isobutyraldehyde, 41.29g of formaldehyde solution with a mass concentration of 40%, and 1.0g of catalyst, and react at a temperature of 70°C for 4h;

[0059] After the reaction was completed, the catalyst was removed by hot filtration, and the organic layer was separated by layers at room temperature;

[0060] The second step: oxidation and esterification reaction:

[0061] Put the organic layer separated in the first step above into a 500mL container, add 150mL of methanol, add 100mL of sodium hydroxide solution with a mass concentration of 40% at a temperature of 40°C, feed oxygen until the pressure is 1Mpa, and stir for 1.5 h, removing formaldehyde and water to obtain methyl hydroxytrimethylacetate.

Embodiment 3

[0063] A synthetic method for methyl hydroxytrimethyl acetate, comprising the following steps:

[0064] The first step: aldol condensation reaction:

[0065] In a 500mL container, put 36.05g of isobutyraldehyde, 41.29g of formaldehyde solution with a mass concentration of 40%, and 0.7g of catalyst, and react at a temperature of 70°C for 3h;

[0066] After the reaction was completed, the catalyst was removed by hot filtration, and the organic layer was separated by layers at room temperature;

[0067] The second step: oxidation and esterification reaction:

[0068] Put the organic layer separated in the first step above into a 500mL container, add 150mL of methanol, add 100mL of sodium hydroxide solution with a mass concentration of 40% at a temperature of 35°C, feed oxygen until the pressure is 0.5Mpa, and stir for 1.5 h, removing formaldehyde and water to obtain methyl hydroxytrimethylacetate.

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Abstract

The invention discloses a method for synthesizing methyl hydroxypivalate, comprising: subjecting formaldehyde and isobutyraldehyde as materials to aldol condensation, oxidization and esterification to synthesize methyl hydroxypivalate, and adding an oxide of at least two of cerium, zirconium, praseodymium, terbium and samarium as a catalyst for aldol condensation; introducing oxygen under alkali conditions for oxidization and esterification reactions. Reaction temperature and reaction pH are optimized, it is possible to effectively shorten reacting time, improving reaction total yield and optimize operability of following reactions, and the method has high economic benefit and a promising industrial popularization prospect.

Description

Technical field: [0001] The invention relates to a method for synthesizing methyl hydroxytrimethyl acetate, belonging to the field of chemical synthesis. Background technique: [0002] Methyl hydroxytrimethylacetate is also known as methyl 2,2-dimethyl-3-hydroxypropionate, methyl hydroxypivalate or methyl hydroxypivalate. Methyl hydroxytrimethyl acetate is an important raw material for the synthesis of liquid crystal materials, pharmaceutical intermediates and dyes. It is widely used in saturated polyester resins, polyurethanes, plasticizers and other fields, and is used as a high-grade raw material for the production of resins, paints and coatings; it It is also an important intermediate for the synthesis of the herbicide clomazone. [0003] At present, there are almost no domestic manufacturers, and most of them rely on imports. The main synthetic methods are as follows: the first one starts with formaldehyde and isobutyraldehyde, and generates 2,2-dimethyl-3-hydroxypropa...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/08C07C69/675C07C45/75C07C47/19C07C59/01C07C51/235B01J23/10
CPCB01J23/002B01J23/10B01J2523/00C07C45/75C07C51/235C07C67/08B01J2523/3712B01J2523/3718B01J2523/3737B01J2523/48B01J2523/3756C07C69/675C07C47/19C07C59/01
Inventor 胡海威丁靓闫永平郑辉严辉
Owner ITIC MEDCHEM CO LTD