29835-28-7Relevant articles and documents
Method for synthesizing acetylenic acid by using terminal alkyne and carbon dioxide
-
Paragraph 0106-0114, (2021/07/24)
The invention belongs to the field of organic synthesis, and particularly relates to a method for synthesizing acetylenic acid by using terminal alkyne and carbon dioxide. The method comprises the experimental steps that alkyne, alkali and a solvent are added into a reaction tube, the alkyne serves as a raw material, the alkali and the solvent provide a strong alkaline environment, CO2 is introduced into a reaction container to form a carbon dioxide atmosphere, heating and stirring reaction are carried out, after the reaction is finished, cooling is carried out to the room temperature, extraction and liquid separation are carried out, a water layer is acidified, then separation and purification are further carried out, and the acetylenic acid compound is obtained. The method is carried out under the conditions of low temperature and normal pressure, does not need to add a metal catalyst, is single in product and convenient to separate, good in substrate applicability and safe and simple to operate, and has potential industrial application prospects and good economic benefits.
Silver Nanoparticles Architectured HMP as a Recyclable Catalyst for Tetramic Acid and Propiolic Acid Synthesis through CO2 Capture at Atmospheric Pressure
Ghosh, Swarbhanu,Ghosh, Aniruddha,Riyajuddin, Sk,Sarkar, Somnath,Chowdhury, Arpita Hazra,Ghosh, Kaushik,Islam, Sk. Manirul
, p. 1055 - 1067 (2020/01/21)
The recent advancement on the tailored synthesis of hypercrosslinked microporous polymer (HMP-2) has assembled significant concentration by the virtue of its adjustable porosity, operative design and absolutely ordering structure. This perfectly structured Ag NPs supported carbocatalyst (Ag-HMP-2) has been synthesized by Friedel-Crafts alkylation between 4,4′-Bis(bromomethyl)-1,1′-biphenyl and carbazole over anhydrous iron(III)chloride catalysis followed by the appending of the silver nanoparticles (Ag NPs) onto the material. The silver nanoparticle was decorated over the HMP-2 to prepare the corresponding catalyst (Ag-HMP-2). The characterization of the newly produced material has been conducted by N2 adsorption/desorption studies, XPS, FE-SEM, transmission electron microscopy (TEM) and Powder X-ray diffraction (PXRD) methods. This microporous catalyst has spectacular activities for the production of tetramic acids from various types of propargylic amine derivatives at 60 °C under atmospheric carbon dioxide pressure. Parallel attempt on fixation of CO2 was executed over terminal alkynes to synthesize propiolic acids under 1 atm pressure. The catalyst (Ag-HMP-2) exhibited sufficient recycling ability for the generation of tetramic acids and propiolic acids up to five catalytic runs without reduction in its catalytic activity.
Preparation method of propiolic acid compounds
-
Paragraph 0049; 0050; 0051, (2017/12/09)
The invention belongs to the technical fields of carbon dioxide activation and conversion and related chemistry, and discloses a preparation method of propiolic acid compounds. The preparation method comprises the following steps: (1) adding a copper catalyst, an additive, an alkali, and solid terminal alkynes into a reactor, adding an organic solvent under the protection of nitrogen gas, and filling CO2 into the reactor; or adding a copper catalyst, an additive, and an alkali into a reactor, adding an organic solvent and liquid terminal alkynes, and filling CO2 into the reactor; (2) sealing the reactor, and placing the reactor in an oil bath to carry out reactions; and (3) after reactions, opening a valve of the reactor to slowly release residual gas in the reactor, transferring the reaction liquid to a one-mouth bottle, carrying out concentration, diluting the concentrate by deionized water, adding n-hexane to carry out extraction, adding hydrochloric acid to carry out acidification, adding diethyl ether to carry out extraction, collecting the organic phase, washing the organic phase by a saturated saline solution, drying the organic phase by anhydrous sodium sulfate, filtering, and removing the solvent in vacuum to obtain the target material. The preparation method has the advantages of low reaction cost, simple experiment operation, mild reaction conditions, and easiness for industrialization.