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Acetynoic acid and preparation method thereof

A technology of alkynoic acid and acetylene, applied in the field of alkynoic acid and its preparation, can solve the problems of long reaction time, increase the complexity of post-processing process, etc., achieve simple post-processing operation, high research value, economic and social environmental benefits, shorten the time The effect of reaction time

Pending Publication Date: 2022-08-09
SHANGHAI ADVANCED RES INST CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] However, currently reported CO 2 Most of the carboxylation reactions with terminal alkynes require the synthesis of high-efficiency catalysts, which increases the complexity of the post-treatment process
At the same time, most of the reports are normal pressure reactions, and the reaction time is relatively long.

Method used

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  • Acetynoic acid and preparation method thereof
  • Acetynoic acid and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0080] The present embodiment provides, the preparation method of phenylpropioic acid, comprises the following steps:

[0081] 1) In the autoclave, add 100 mg of dried 4A molecular sieves, 2 mmol of phenylacetylene, 2.4 mmol of cesium carbonate and 6 mL of anhydrous dimethyl sulfoxide.

[0082] 2) After sealing the autoclave, fill it with carbon dioxide gas, and then empty it. The replacement gas operation was repeated 6 times to ensure that no air remained in the reactor.

[0083] 3) Then charged with 0.1Mpa carbon dioxide, raised to 70°C and reacted for 20h.

[0084] 4) After cooling the reaction product obtained in 3) to room temperature, remove the 4A molecular sieve, then add water with a volume ratio of 1:1 to dimethyl sulfoxide for mixing, continue stirring for 30 min, and extract 4 times with dichloromethane, The first aqueous phase was obtained; the first aqueous phase was cooled in an ice-water bath, acidified to pH 1 with HCl (V / V=1:1), and extracted four times wi...

Embodiment 2

[0088] The present embodiment provides, the preparation method of phenylpropioic acid, comprises the following steps:

[0089] 1) In the autoclave, add 100 mg of dried 4A molecular sieves, 2 mmol of phenylacetylene, 2.4 mmol of cesium carbonate and 6 mL of anhydrous dimethyl sulfoxide.

[0090] 2) After sealing the autoclave, fill it with carbon dioxide gas, and then empty it. The replacement gas operation was repeated 6 times to ensure that no air remained in the reactor.

[0091] 3) Then charged with 0.1Mpa carbon dioxide, raised to 40°C and reacted for 20h.

[0092] 4) After cooling the reaction product obtained in 3) to room temperature, remove the 4A molecular sieve, then add water with a volume ratio of 1:1 to dimethyl sulfoxide for mixing, continue stirring for 30 min, and extract 4 times with dichloromethane, The first aqueous phase was obtained; the first aqueous phase was cooled in an ice-water bath, acidified to pH 1 with HCl (V / V=1:1), and extracted four times wi...

Embodiment 3

[0095] The present embodiment provides, the preparation method of phenylpropioic acid, comprises the following steps:

[0096] 1) In the autoclave, add 100 mg of dried 4A molecular sieves, 2 mmol of phenylacetylene, 2.4 mmol of cesium carbonate and 6 mL of anhydrous dimethyl sulfoxide.

[0097] 2) After sealing the autoclave, fill it with carbon dioxide gas, and then empty it. The replacement gas operation was repeated 6 times to ensure that no air remained in the reactor.

[0098] 3) Then charged with 0.1Mpa carbon dioxide, raised to 50°C and reacted for 20h.

[0099] 4) After cooling the reaction product obtained in 3) to room temperature, remove the 4A molecular sieve, then add water with a volume ratio of 1:1 to dimethyl sulfoxide for mixing, continue stirring for 30 min, and extract 4 times with dichloromethane, The first aqueous phase was obtained; the first aqueous phase was cooled in an ice-water bath, acidified to pH 1 with HCl (V / V=1:1), and extracted four times wi...

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Abstract

The invention belongs to the field of organic synthesis, and discloses an acetylenic acid and a preparation method thereof, the method comprises the following steps: 1) placing a molecular sieve, an auxiliary agent alkali and terminal alkyne in a carbon dioxide atmosphere, and carrying out a reaction; (2) mixing the obtained reaction product with an inorganic solvent, and extracting by adopting an extracting agent to obtain a water phase; and (3) acidifying the water phase, then carrying out impurity removal and extraction, namely carrying out extraction procedures for at least three times to obtain an organic phase, drying the organic phase, and then carrying out solid-liquid separation to obtain the acetylenic acid. According to the method, CO2 and terminal alkyne are directly carboxylated to prepare acetylenic acid, CO2 can be effectively utilized, the problems that a traditional acetylenic acid industrial preparation method is tedious in process, unfriendly to the environment and the like can be solved, and the method has high research value and economic and social environmental benefits.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to an alkynoic acid and a preparation method thereof. Background technique [0002] carbon dioxide (CO 2 ) excessive emissions lead to a severe greenhouse effect, but CO 2 At the same time, it is also a safe, non-toxic, cheap and easily available carbon resource with abundant reserves. chemically convert CO 2 The conversion into chemicals with high added value is of great significance. Among them, the use of CO 2 Synthesis of alkynes, which are CO 2 an important aspect of exploitation. [0003] Although currently in CO 2 A lot of research work has been carried out on the chemical conversion and utilization of chemistry, and gratifying progress has been made (P.Gao, et al., Nat.Chem., 2017, 9(10), 1019.J.W.Zhong, et al., Chem.Soc. .Rev., 2020, 49(5), 1385.), but a lot of CO 2 The reactions involved have not yet been industrialized. [0004] Research on efficient and reasona...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/15C07C57/42C07C51/48
CPCC07C51/15C07C51/48C07C57/42
Inventor 张莉娜孙楠楠史佳林魏伟
Owner SHANGHAI ADVANCED RES INST CHINESE ACADEMY OF SCI
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