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Process for synthesizing ethyl propiolate

A technique for the synthesis of ethyl propiolate and its synthesis method, applied in the field of synthesis of ethyl propiolate, capable of solving problems such as operational hazards, environmental pollution, complex reaction systems, etc., achieving mild reaction conditions, no pollution to the environment, and easy availability of raw materials Effect

Inactive Publication Date: 2008-12-10
SUZHOU YUANFANG CHEM
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Problems solved by technology

[0008] Taking a broad view of the above four methods, method 1 will produce a large amount of chromium sulfate waste liquid, which will pollute the environment; method 2 needs to use metallic sodium, and is carried out in a pressure vessel, which is dangerous to operate and poor in safety; method 3 has a complex reaction system and low yield. Low; method 4 has high raw material cost and is not competitive
[0009] In the prior art, ethyl propiolate is obtained by the esterification reaction of propiolic acid and ethanol under the action of a catalyst, wherein the catalyst includes sulfuric acid, boron trifluoride ethyl ether, etc., and the former, due to the use of a large amount of sulfuric acid, will The environment causes pollution, while the latter has problems such as high cost

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  • Process for synthesizing ethyl propiolate
  • Process for synthesizing ethyl propiolate
  • Process for synthesizing ethyl propiolate

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Embodiment Construction

[0020] The synthetic route of the present invention is:

[0021]

[0022] The possible mechanism of the method is: calcium hypochlorite reacts with acetic acid to generate oxidative hypochlorous acid, the hypochlorous acid preferentially oxidizes propynyl alcohol to generate propiole aldehyde, and propiole aldehyde is further converted into ethyl propiolate.

[0023] The present invention will be described in detail below in conjunction with specific embodiments.

[0024] In a 500mL reaction flask, put 230ml of dichloromethane, 56g of propynyl alcohol, 138g of absolute ethanol, 360g of glacial acetic acid, 429g of calcium hypochlorite and 20g of molecular sieves, and stir at room temperature. GC followed until the starting material was reacted to completion. After the reaction, add 300ml of water and 10g of sodium thiosulfate and stir for half an hour, then slowly add solid sodium bicarbonate to adjust the pH to 7-8. Stand to separate the layers, extract the aqueous phase...

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Abstract

The invention relates to a method for synthesizing ethyl propiolate, comprising the following steps of: using propargyl alcohol and ethanol as reaction raw materials; using dichloromethane as a solvent with a reaction temperature between 0 and 40 DEG C; and carrying out a one-step synthesis of the ethyl propiolate by using the reaction raw materials under actions of calcium hypochlorite and an acetic acid. The method has the advantages of easy acquisition of raw materials, convenient method, mild reaction conditions and no pollution to environment, and is capable of performing the reaction under a room temperature.

Description

technical field [0001] The present invention relates to a kind of synthetic method of ethyl propiolate. Background technique [0002] Ethyl propiolate is an important organic chemical raw material and pharmaceutical intermediate. In the prior art, propynyl alcohol is used as raw material, and propiolate is obtained by esterification after oxidation to propiolic acid. [0003] The synthesis of propiolic acid mainly has the following methods: [0004] 1. Utilize the sulfuric acid solution of chromium trioxide to oxidize propynyl alcohol to propiolic acid. [0005] 2. US2786022 reported that sodium acetylide was reacted with carbon dioxide in an autoclave to obtain sodium propiolate and then acidified to obtain propiolic acid. [0006] 3. US20040059154 and US20030158439 report the oxidation of propynol to propiolic acid using sodium hypochlorite under the catalysis of 4-hydroxy-TEMPO. [0007] 4. Obtaining propiolic acid through decarboxylation of butynedioic acid monosodiu...

Claims

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Application Information

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IPC IPC(8): C07C69/606C07C67/08
Inventor 邹贵祥陈智浩刘宏元
Owner SUZHOU YUANFANG CHEM
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