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A kind of technology of synthesizing methylparaben

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: 2022-08-09
JIANGSU JIYI NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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 acylation, halogenation, hydrolysis, reaction yield is low, operation is complicated, and a large amount of waste water is produced simultaneously, easy to pollute the environment

Method used

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  • A kind of technology of synthesizing methylparaben
  • A kind of technology of synthesizing methylparaben

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Preparation of methyl parahydroxyphenylpropionate: 500 g of liquid methyl 3-(3,5-di-tert-butyl-4-hydroxy) phenylpropionate with a temperature of 100°C was continuously passed through an advection pump with a flow rate of 4ml / min Add dropwise to the reactor containing 1.0 g of phosphotungstic acid catalyst and carry out stirring reaction at a temperature of 115 ° C (chemical reaction formula such as figure 1 shown), generate product methyl parahydroxybenzoate and by-product isobutylene, and 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 reaction kettle is about 100g, and the reflux ratio at the top of the rectification tower is controlled to be 1:1. Extracted from the top of the rectifying tower, the remaining part of methylparaben and methyl 3-(3,5-di-tert-butyl-4-hydroxy)phenylpropionate are retu...

Embodiment 2

[0031] Preparation of methyl parahydroxyphenylpropionate: 500 g of liquid methyl 3-(3,5-di-tert-butyl-4-hydroxy) phenylpropionate with a temperature of 100°C was continuously passed through an advection pump with a flow rate of 5ml / min Add dropwise to the reaction kettle containing phosphotungstic acid catalyst 1.0g and carry out stirring reaction at a temperature of 125 ° C to generate product methylparaben and by-product isobutene, and the material in the reaction kettle is distilled by a rectifying tower, The temperature at the top of the rectifying tower is 111°C, the pressure of the reaction kettle and the rectifying tower is -1kpa, the weight of the material in the reaction kettle after the reaction is stable is about 100g, and the reflux ratio of the control tower top of the rectifying tower is 1.5:1, The materials in the reaction kettle are continuously extracted through the top of the rectification tower; after the complete reaction, the reflux ratio of the top of the ...

Embodiment 3

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

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Abstract

The invention discloses a process for synthesizing methyl p-hydroxyphenylpropionate, which is catalyzed by 3-(3,5-di-tert-butyl-4-hydroxy) methyl phenylpropionate raw material and an acid catalyst, and is catalyzed in a reaction distillation kettle Continuous reactive distillation is carried out to obtain methylparaben. The technological process of the invention makes the raw materials fully utilized, the catalyst consumption is small, the production process is simple, and the operation is convenient; at the same time, the generated by-product isobutene can be recovered and can be used as German raw materials for other products, so that no three wastes are generated in the whole technological process, It is an environment-friendly process; the methylparaben prepared by the synthesis process has a high yield and excellent quality, and has good industrial production value.

Description

technical field [0001] The invention relates to a process for synthesizing methyl parahydroxyphenylpropionate, and belongs to the technical field of fine chemicals. Background technique [0002] Methylparaben is an important organic fine chemical intermediate, which can synthesize various compounds such as stabilizers, colorants, optical materials, and is also an important pharmaceutical intermediate. Methylparaben is used in the preparation of hydrochloric acid. An important intermediate for esmolol. [0003] At present, it is said that the reported synthetic route of methyl p-hydroxyphenylpropionate, the synthetic routes in the documents such as patent CN1200367A, CN108640834A and Shinde need steps such as acylation, halogenation, hydrolysis, etc., the reaction yield is low, the operation is complicated, and a large amount of waste water is generated at the same time, It is easy to cause pollution to the environment. [0004] Therefore, in order to reduce the production ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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