Synthesis process of methyl 3-(3-tert-butyl-4-hydroxy) phenylpropionate

A technology of methyl hydroxyphenylpropionate and methyl phenylpropionate, which is applied in the field of synthesis of methyl 3-phenylpropionate, can solve the problems of non-reusable catalysts, increased economic costs, and many by-products, and achieves The effect of good industrial production value, excellent quality and high utilization rate

Inactive Publication Date: 2021-03-12
JIANGSU JIYI NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In this process, the catalyst cannot be reused; moreover, due to the catalyst activity and selectivity, there are many by-products, and the reaction yield is 75%-85%, resulting in waste of raw materials and increasing economic costs

Method used

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  • Synthesis process of methyl 3-(3-tert-butyl-4-hydroxy) phenylpropionate
  • Synthesis process of methyl 3-(3-tert-butyl-4-hydroxy) phenylpropionate

Examples

Experimental program
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Effect test

Embodiment 1

[0024] (1) Preparation of 3-(3-tert-butyl-4-hydroxyl) methyl phenylpropionate: 200 g of methyl p-hydroxyphenyl propionate and 58 g of tert-butanol (molar ratio is 1:0.7) are added to a temperature of Mix evenly in a pre-mixing tank at 40-45°C, and continuously add it to a column-and-tube fixed-bed reactor filled with granular solid sulfonic acid resin at a temperature of 100°C, an inner diameter of 2cm, and a packing height of 100cm through an advection pump with a flow rate of 2ml / min. The reaction is carried out in the tubular fixed bed reactor, and the average residence time of the material in the tubular fixed bed reactor is 1.04h. The thick product of methyl p-hydroxyphenylpropionate; sample is taken at the outlet of the reactor, and quantitatively analyzed by gas chromatography, the conversion rate of methyl p-hydroxyphenylpropionate is 63.31%, the conversion rate of tert-butyl alcohol is 91.02%, and the by-product 3-(35-di-tert-butyl The content of methyl-4-hydroxy)phen...

Embodiment 2

[0027] (1) Preparation of 3-(3-tert-butyl-4-hydroxyl) methyl phenylpropionate: 200 g of methyl p-hydroxyphenyl propionate and 58 g of tert-butanol (molar ratio is 1:0.7) are added to a temperature of Mix evenly in a pre-mixing tank at 40-45°C, and continuously add it to the column-and-tube fixed-bed reaction of packing granular solid sulfonic acid resin at a temperature of 100°C, an inner diameter of 2cm, and a packing height of 100cm through an advection pump with a flow rate of 1.5ml / min. The reaction is carried out in the reactor, and the average residence time of the material in the tubular fixed-bed reactor is 1.39h, and flows out from the outlet of the tubular fixed-bed reactor to obtain 3-(3-tert-butyl-4-hydroxyl)benzene The crude product of methyl propionate; sample is taken at the outlet of the reactor, and quantitatively analyzed by gas chromatography, the conversion rate of methyl p-hydroxyphenylpropionate is 63.97%, the conversion rate of tert-butyl alcohol is 92.13...

Embodiment 3

[0030](1) Preparation of 3-(3-tert-butyl-4-hydroxyl) methyl phenylpropionate: 200 g of methyl p-hydroxyphenyl propionate and 58 g of tert-butanol (molar ratio is 1:0.7) are added to a temperature of Mix evenly in a pre-mixing tank at 40-45°C, and continuously add it to a column-and-tube fixed-bed reactor filled with granular solid sulfonic acid resin at a temperature of 100°C, an inner diameter of 2cm, and a packing height of 100cm through an advection pump with a flow rate of 1ml / min. The reaction is carried out in the tubular fixed-bed reactor, and the average residence time of the material in the tubular fixed-bed reactor is 2.08h, and flows out from the outlet of the tubular fixed-bed reactor to obtain 3-(3-tert-butyl-4-hydroxyl) phenylpropane The crude product of methyl p-hydroxyphenyl propionate; sample is taken at the outlet of the reactor, and quantitatively analyzed by gas chromatography, the conversion rate of methyl p-hydroxyphenylpropionate is 63.97%, the conversion...

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Abstract

The invention discloses a synthesis process of methyl-3-(3-tert-butyl-4-hydroxy) phenylpropionate, which comprises the following steps of mixing methyl p-hydroxyphenylpropionate and tert-butyl alcoholaccording to a certain molar ratio, and carrying out continuous reaction in a tubular fixed bed reactor filled with a solid catalyst to obtain a crude product of methyl 3-(3-tert-butyl-4-hydroxy) phenylpropionate, and distilling to remove water with a low boiling point, carrying out secondary separation on residual tert-butyl alcohol through a rectifying tower to obtain a methyl 3-(3-tert-butyl-4-hydroxy) phenylpropionate product. According to the synthesis process, methyl p-hydroxyphenylpropionate and tert-butyl alcohol are used as raw materials, granular solid sulfonic acid resin is used, continuous reaction is performed, secondary separation is performed through a rectifying tower, a high-purity methyl 3-(3-tert-butyl-4-hydroxy) phenylpropionate product is obtained, the yield is high,the quality is excellent, unreacted methyl p-hydroxyphenyl propionate is recycled, so that the method has good industrial production value, and the production cost is reduced.

Description

technical field [0001] The invention relates to a synthesis process of methyl 3-(3-tert-butyl-4-hydroxy)phenylpropionate, which belongs to the technical field of fine chemicals. Background technique [0002] 3-(3-tert-butyl-4-hydroxy)methyl phenylpropionate is an important organic fine chemical intermediate, due to its unique structure, it is a hindered phenol, because there is a tert-butyl group in the ortho position It has a protective effect on the phenolic hydroxyl groups of hindered phenols, and can prevent the phenols from self-oxidative loss. Compared with simple phenols, the antioxidant performance is significantly improved; It has strong activity, can carry out various chemical reactions, and can synthesize various compounds such as stabilizers, colorants, optical materials and pharmaceutical intermediates, etc., and has been widely used in polymer materials, printing, auxiliary agents, dyes, pharmaceuticals and other industries. 3-(3-tert-butyl-4-hydroxy)methyl ph...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/343C07C69/732C07C67/54
CPCC07C67/343C07C67/54
Inventor 郭骄阳赵崇鑫陈芬儿程荡黄则度肖霄
Owner JIANGSU JIYI NEW MATERIAL CO LTD
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