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Environment-friendly preparation method of propiolic acid derivatives

A technology of propynoic acid and derivatives is applied in the field of compound preparation, which can solve the problems of high safety risk and large environmental pollution, and achieve the effects of high operational safety, little environmental pollution and convenient operation.

Inactive Publication Date: 2020-01-17
安庆博曼生物技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0012] Aiming at the environmental pollution of the reported propiolic acid synthesis method, the problem of high safety risk, the present invention at first provides a kind of environmentally friendly, new propiolic acid synthesis method with high safety factor; on this basis, the present invention further Provided is a method for synthesizing methyl propiolate and ethyl propiolate with less alcohol consumption, complete reaction, high yield and easy separation

Method used

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  • Environment-friendly preparation method of propiolic acid derivatives

Examples

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Effect test

Embodiment 1

[0044] Embodiment one: the preparation of dipotassium salt of butynedioic acid

[0045] In a 2L three-neck flask, equipped with a thermometer and a condenser, put 417g of water and 60g of potassium hydroxide into it, and stir to dissolve it. At a temperature of 60°C, add 50g of 2,3-dibromosuccinic acid several times to control the temperature below 100°C. , The addition was completed in about 2 hours; heating and holding at 80°C, and reacting for 10 hours, the reaction of the raw materials was detected by HPLC, and it was set aside.

Embodiment 2

[0046] Example 2: Preparation of butynedioic acid disodium salt

[0047] In a 2L three-neck flask, equipped with a thermometer and a condenser, put 417g of water and 43g of sodium hydroxide into it, and stir to dissolve it. At a temperature of 60°C, add 50g of 2,3-dibromosuccinic acid several times to control the temperature below 100°C. The addition is completed in about 2 hours; heat and keep warm at 80°C, and react for 10 hours. The reaction of the raw materials is detected by HPLC, and it is set aside.

Embodiment 3

[0048] Embodiment three: the preparation of butynedioic acid dipotassium salt

[0049] In a 2L three-neck flask, equipped with a thermometer and a condenser, put 1000g of methanol and 60g of potassium hydroxide into it, and stir to dissolve it. At a temperature of 60°C, add 50g of 2,3-dibromosuccinic acid at one time, reflux, and react for 24 hours. The reaction of the raw materials was detected by HPLC, cooled to room temperature, and suction filtered to obtain 92 g of dipotassium butynedioic acid and potassium bromide mixture for subsequent use.

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Abstract

The invention discloses an environment-friendly preparation method of propiolic acid derivatives. The preparation method comprises the following steps: (1) with 2,3-dibromosuccinic acid as a raw material, generating a butynedioic acid salt under alkaline conditions; (2) under an acidic condition, carrying out high-temperature decarboxylation to obtain propiolic acid; and (3) adding corresponding methanol or ethanol into propiolic acid in an extraction solvent, and preparing high-yield propiolate under acidic catalytic conditions under the condition that trimethyl orthoformate or triethyl orthoformate participates in dehydration. In the invention, the propiolic acid preparation method is friendly to environment and high in safety coefficient; and the method provided by the invention can beused for preparing methyl propiolate and ethyl propiolate, and has the advantages of small alcohol consumption, thorough reaction, high yield and easiness in separation.

Description

technical field [0001] The invention relates to the technical field of compound preparation, more specifically to a preparation method of propiolic acid derivatives. Background technique [0002] Propiolic acid derivatives such as methyl propiolate and ethyl propiolate are important fine chemicals used as additives in electroplating solution formulations, intermediates in organic synthesis of drugs and functional materials. For organic synthesis, it can be used to prepare propionic acid, trimesic acid, halogenated acrylic acid, dihalogenated acrylic acid, diacetylene dicarboxylic acid, ethyl propiolate, pyrazolone, dibromocrotonic acid, ethoxy crotonic acid etc. Methyl propiolate can be prepared by heating propiolic acid with sulfuric acid and methanol under reflux, which is the raw material of antiviral drug iodine. [0003] There are two traditional preparations of propiolic acid: one is obtained by oxidation of propynyl alcohol, and propynyl alcohol is added to acetone ...

Claims

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Application Information

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IPC IPC(8): C07C67/08C07C69/606C07C51/41C07C57/22C07C57/20C07C51/38
CPCC07C51/38C07C51/412C07C67/08C07C57/22C07C57/20C07C69/606
Inventor 陈佳何雪垠刘腾蛟
Owner 安庆博曼生物技术有限公司
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