1483-67-6Relevant articles and documents
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Khan,G.R. et al.
, p. 215 - 216 (1979)
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Wotiz et al.
, p. 1221 (1956)
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Haynes,Jones
, p. 503,505 (1946)
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Microwave-assisted fabrication of a mixed-ligand [Cu4(μ3-OH)2]-cluster-based metal–organic framework with coordinatively unsaturated metal sites for carboxylation of terminal alkynes with carbon dioxide
Wang, Wen-Jing,Sun, Zhong-Hua,Chen, Sheng-Chun,Qian, Jun-Feng,He, Ming-Yang,Chen, Qun
, (2021/05/24)
The development of efficient and stable metal–organic framework (MOF) catalysts with coordinatively unsaturated metal sites for modern organic synthesis is greatly important. Herein, a robust [Cu4(μ3-OH)2]-cluster-based MOF (Cu-MOF) with a mixed-ligand system was successfully fabricated by a microwave-assisted method under mild conditions. The as-prepared Cu-MOF catalyst possessing unsaturated Cu (II) sites exhibited excellent catalytic activity toward the direct carboxylation of 1-ethynylbenzene with CO2, and various propiolic acid derivatives were synthesized in moderate to good yields under optimized reaction conditions. Furthermore, the catalyst remained stable and could be easily recycled for five sequential runs without incredible decrease in catalytic efficiency.
Method for rapidly preparing acetylenic acid and derivatives thereof based on microchannel continuous flow technology
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Paragraph 0027, (2021/05/19)
The invention discloses a method for rapidly preparing acetylenic acid and derivatives thereof based on a microchannel continuous flow technology. The method comprises a lithium-hydrogen exchange reaction and a nucleophilic addition reaction. The lithium-hydrogen exchange reaction comprises the following steps: pumping a terminal alkyne solution and a butyl lithium solution into a first-section microchannel reactor according to a certain equivalent proportion, and carrying out the lithium-hydrogen exchange reaction at a certain temperature for a certain time to generate terminal alkynyl lithium. The nucleophilic addition reaction comprises the following steps: introducing the terminal alkynyl lithium obtained in the lithium hydrogen exchange reaction into a second-section micro-channel reactor, mixing the terminal alkynyl lithium with CO2 gas with a certain equivalent proportion, carrying out reacting for a certain period of time at a certain temperature to generate terminal alkynyl carboxylic acid lithium salt, and acidifying the product to obtain a terminal alkynyl carboxylic acid product. The synthesis method provided by the invention is friendly to environment, high in efficiency, low in cost, mild in conditions and good in substrate universality in virtue of a coupling micro-channel continuous flow technology. According to the invention, the danger coefficient of the lithium-containing reagent is greatly reduced, so the reactions can achieve higher product purity under a controllable continuous condition.
Structural Elucidation of Trace Components Combining GC/MS, GC/IR, DFT-Calculation and Synthesis—Salinilactones, Unprecedented Bicyclic Lactones from Salinispora Bacteria
Schlawis, Christian,Kern, Simone,Kudo, Yuta,Grunenberg, J?rg,Moore, Bradley S.,Schulz, Stefan
supporting information, p. 14921 - 14925 (2018/10/24)
The analysis of volatiles released by marine Salinispora bacteria uncovered a new class of natural compounds displaying an unusual bicyclic [3.1.0]-lactone skeleton. Although only sub-μg quantities of the compounds were available, the combination of analytical methods, computational spectroscopy, and synthesis allowed unambiguous structural identification of the compounds, called salinilactones, without the need for isolation. Orthogonal hyphenated methods, GC/MS and solid-phase GC/IR allowed to propose a small set of structures consistent with the data. A candidate structure was selected by comparison of DFT-calculated IR spectra and the experimental IR-spectrum. Synthesis confirmed the structure and absolute configuration of three bicyclic lactones, salinilactones A–C. The salinilactones are structurally closely related to the A-factor class of compounds, autoregulators from streptomycete bacteria. They exhibited inhibitory activity against Salinispora and Streptomyces strains.
