Process for synthesizing methyl p-hydroxyphenylpropionate

A technology for methyl hydroxyphenylpropionate and methyl phenylpropionate is applied in the field of synthesizing methyl parahydroxyphenylpropionate, can solve problems such as low reaction yield, waste water generation, environmental pollution, etc., and achieves simple production process and easy operation. Convenience and the effect of less catalyst consumption

Active Publication Date: 2021-04-02
JIANGSU JIYI NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, the synthetic route of methyl p-hydroxyphenylpropionate reported, the synthetic route in patents CN1200367A, CN108640834A and Shinde etc. need steps such as ac

Method used

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  • Process for synthesizing methyl p-hydroxyphenylpropionate
  • Process for synthesizing methyl p-hydroxyphenylpropionate

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Preparation of methyl p-hydroxyphenylpropionate: 500g of liquid 3-(3,5-di-tert-butyl-4-hydroxy)methyl phenylpropionate at a temperature of 100°C was continuously Add dropwise to the reaction kettle containing 1.0g of phosphotungstic acid catalyst and carry out stirring reaction at a temperature of 115°C (the chemical reaction formula is as follows figure 1 Shown), generate product methyl p-hydroxyphenylpropionate and by-product isobutylene, and the material in the reactor is distilled by rectifying tower, the temperature of rectifying tower tower top is 105 ℃, and the pressure of reactor and rectifying tower is- 1kpa, after the reaction is stable, the material in the reactor is about 100g, the reflux ratio at the top of the rectification tower is controlled to be 1:1, the material in the reactor is continuously extracted through the top of the rectification tower, part of methyl p-hydroxyphenylpropionate and isobutyl Extracted from the top of the rectifying tower, the r...

Embodiment 2

[0031] Preparation of methyl p-hydroxyphenylpropionate: 500g of liquid 3-(3,5-di-tert-butyl-4-hydroxy)methyl phenylpropionate at a temperature of 100°C is continuously Add it dropwise to a reaction kettle containing 1.0g of phosphotungstic acid catalyst and carry out a stirring reaction at a temperature of 125°C to generate the product methyl p-hydroxyphenylpropionate and by-product isobutylene, and the materials in the reaction kettle are distilled through a rectification tower. The temperature at the top of the rectifying tower is 111°C, the pressure of the reactor and the rectifying tower is -1kpa, the weight of the material in the reactor is about 100g after the reaction is stable, and the reflux ratio at the top of the rectifying tower is controlled to be 1.5:1. The materials in the reactor are continuously extracted through the top of the rectification tower; after complete reaction, the reflux ratio of the top of the rectification tower is maintained, and the materials i...

Embodiment 3

[0034] Preparation of methyl p-hydroxyphenylpropionate: 500g of liquid methyl 3-(3,5-di-tert-butyl-4-hydroxy)phenylpropionate at a temperature of 100°C is continuously passed through a flow pump with a flow rate of 6ml / min Add it dropwise into a reaction kettle containing 1.0g of phosphotungstic acid catalyst and carry out a stirring reaction at a temperature of 135°C to generate the product methyl p-hydroxyphenylpropionate and by-product isobutylene, and the materials in the reaction kettle are distilled through a rectification tower. The temperature at the top of the rectification tower is 115°C, the pressure of the reactor and the rectification tower is -1kpa, the weight of the material in the reactor after the reaction is stable is about 100g, and the reflux ratio at the top of the rectification tower is controlled to be 2:1. The materials in the reactor are continuously extracted through the top of the rectification tower; after complete reaction, the reflux ratio of the t...

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Abstract

The invention discloses a process for synthesizing methyl p-hydroxyphenylpropionate. The process comprises the following steps of: catalyzing a 3-(3, 5-di-tert-butyl-4-hydroxy) methyl phenylpropionateraw material by using an acid catalyst, and carrying out continuous reaction rectification in a reaction rectification kettle to obtain the methyl p-hydroxyphenylpropionate. According to the technological process, raw materials are fully utilized, the catalyst dosage is small, the production technology is simple, and operation is convenient; meanwhile, the generated by-product isobutene is recycled and can be used as a German raw material of other products, so that no three wastes are generated in the whole technological process, and the process is an environment-friendly process; the methylp-hydroxyphenylpropionate prepared by the synthesis process is relatively high in yield and excellent in quality, and has a very good industrial production value.

Description

technical field [0001] The invention relates to a process for synthesizing methyl p-hydroxyphenylpropionate, which belongs to the technical field of fine chemicals. Background technique [0002] Methyl p-hydroxyphenylpropionate is an important organic fine chemical intermediate, which can synthesize a variety of compounds such as stabilizers, colorants, optical materials, and is also an important pharmaceutical intermediate. Methyl p-hydroxyphenylpropionate is used to prepare hydrochloric acid An important intermediate of Esmolol. [0003] At present, the synthetic route of methyl p-hydroxyphenylpropionate reported, the synthetic route in patents CN1200367A, CN108640834A and Shinde etc. need steps such as acylation, halogenation, hydrolysis, reaction yield is low, operation is complicated, and a large amount of waste water is produced simultaneously, It is easy to pollute the environment. [0004] Therefore in order to reduce production costs, avoid raw material loss, and ...

Claims

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Application Information

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IPC IPC(8): C07C67/333C07C67/54C07C69/732
CPCC07C67/333C07C67/54C07C69/732Y02P20/10
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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