- Method for preparing olefine aldehyde by catalyzing terminal alkyne or terminal conjugated eneyne and diphosphine ligand used in method
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The invention discloses a method for preparing olefine aldehyde by catalyzing terminal alkyne or terminal conjugated eneyne and a diphosphine ligand used in the method. According to the invention, indole-substituted phosphoramidite diphosphine ligand which is stable in air and insensitive to light is synthesized by utilizing a continuous one-pot method, and the indole-substituted phosphoramidite diphosphine ligand and a rhodium catalyst are used for jointly catalyzing to successfully achieve a hydroformylation reaction of aromatic terminal alkyne and terminal conjugated eneyne under the condition of synthesis gas for the first time, so that an olefine aldehyde structure compound can be rapidly and massively prepared, and particularly, a polyolefine aldehyde structure compound which is more difficult to synthesize in the prior art can be easily prepared and synthesized, and a novel method is provided for synthesis and modification of drug molecules, intermediates and chemical products.
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Paragraph 0126-0131
(2021/05/29)
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- Preparation method of P-tert-butylphenylpropionaldehyde
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The invention relates to a preparation method of p-tert-butyl phenylpropionaldehyde. The preparation method comprises the following steps: subjecting p-tert-butylbenzaldehyde, alkyl orthoformate and afirst catalyst to mixing and a reaction, then adding vinyl ether, carrying out mixing and a reaction, then adding a second catalyst and a second solvent, performing a hydrolysis reaction, and finallysubjecting obtained supernatant containing a reaction product to catalytic hydrogenation to obtain p-tert-butylphenylpropionaldehyde. Through selection of a specific catalyst, the multi-step reactions of the method provided by the invention can be continuously carried out; separation and extraction of an intermediate product are not needed; the multi-step reactions can be realized in one reactionsystem; according to a technical scheme provided by the invention, the product is prepared from the raw materials through one-pot reactions, and reaction conditions are mild; and the obtained p-tert-butylphenylpropionaldehyde has a content of 70% or above, is colorless transparent oily liquid, and can be directly used for essence preparation, and the highest yield can reach 93.1%.
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- Evolution of physical and photocatalytic properties of new Zn(II) and Ru(II) complexes
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Synthesis of Zn(II) and Ru(II) complexes were reported by using N4-macrocyclic Schiff base ligands under solvothermal conditions. The newly synthesized Zn(II) and Ru(II) complexes have been characterized by various physico-chemical techniques such as elemental analysis, molar conductance, HRMS, TGA, FESEM, UV–Vis, FT-IR, 1H NMR, and cyclic voltammetry. By using molar conductance studies, the complexes are formulated as [Zn(TPTTP)]Cl2 and [Ru(TPTTP)Cl2]. C–H bond activation of an sp3 group of methylstyrenes (converted into cinnamaldehydes) and C–H bond activation of the sp2 bond of polycyclic aromatic hydrocarbons through photooxidation was examined in the presence of Zn(II) and Ru(II) complexes. Reusable activity studies and photostability of catalyst are investigated by using UV–Vis spectra. Based on the results, higher catalytic activity of [Ru(TPTTP)Cl2] complex than [Zn(TPTTP)]Cl2 complex in both C–H bond activation and photooxidation of aromatic hydrocarbons has been reported.
- Gugulothu, Venkanna,Ahemed, Jakeer,Subburu, Mahesh,Yadagiri, Bhongiri,Mittal, Ritu,Prabhakar, Chetti,Pola, Someshwar
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p. 412 - 423
(2019/06/27)
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- Palladium-Catalyzed Cascade Double C—N Bond Activation: A New Strategy for Aminomethylation of 1,3-Dienes with Aminals
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A new palladium-catalyzed selective aminomethylation of conjugated 1,3-dienes with aminals via double C—N bond activation is described. This simple method provides an effective and rapid approach for the synthesis of linear α,β-unsaturated allylic amines with perfect regioselectivity. Mechanistic studies disclosed that one palladium catalyst cleaved two distinct C—N bond to furnish a cascade double C—N bond activation, in which an allylic 1,3-diamine and allylic 1,2-diamine were initially formed as key intermediates through the palladium-catalyzed C—N bond activation of aminal and the α,β-unsaturated allylic amine was subsequently produced via palladium-catalyzed C—N bond activation of the allylic diamines.
- Qiao, Cuifang,Chen, Anrong,Gao, Bingjian,Liu, Yang,Huang, Hanmin
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supporting information
p. 929 - 933
(2018/09/22)
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- Method for synthesizing 3-(4-tert-butylphenyl)propionaldehyde
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The invention discloses a method for synthesizing 3-(4-tert-butylphenyl)propionaldehyde. The method is executed according to reaction formulas as shown in the description and specifically comprises following steps: a compound shown as the formula I is subjected to Claisen-Schmidt condensation reaction, unsaturated aldehydes are produced, and a compound shown as the formula II is obtained; the compound shown as the formula II is dissolved in toluene and ethanediol and subjected to fractional distillation and water discharge under the action of a catalyst, and a compound shown as the formula IIIis produced through condensation; the compound shown as the formula III is dissolved in a solvent, then the catalyst is added, hydrogen is introduced under pressurizing action to reduce double bonds,and a compound shown as the formula IV is obtained; acetal shown as the formula IV is hydrolyzed under the acidic condition to form aldehyde, and 3-(4-tert-butylphenyl)propionaldehyde shown as the formula V is obtained. Compared with Friedel-Crafts acylation reaction in the prior art, the method for synthesizing 3-(4-tert-butylphenyl)propionaldehyde has the advantages as follows: conditions are mild, the Claisen-Schmidt condensation reaction is high in selectivity, unicity of condensation is high, and the problem of severe pollution caused by high consumption of strong-corrosion titanium tetrachloride is solved. The reaction synthesis is low-pollution, aftertreatment is simple, and the requirement of modern green production is met.
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Paragraph 0015; 0016-0019; 0020-0021
(2018/05/16)
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- Tricyclohexylphosphine-Catalyzed Cycloaddition of Enynoates with [60]Fullerene and the Application of Cyclopentenofullerenes as n-Type Materials in Organic Photovoltaics
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The tricyclohexylphosphine-catalyzed [3 + 2] cycloaddition of (E)-alkyl 5-substituted phenylpent-4-en-2-ynoates with [60]fullerene was studied. This reaction undergoes an initial 1,3-addition of phosphines toward the α-carbons of enynoates. Subsequent cycloaddition of the generated 1,3-dipoles with [60]fullerene and elimination of tricyclohexylphosphines resulted in cyclopentenofullerenes in 20-43% yields. The isolated cyclopentenofullerenes were observed to serve as n-type materials in organic photovoltaics, providing a maximum average power conversion efficiency of 3.79 ± 0.29% upon embedding with P3HT in the active layer.
- Wu, An-Ju,Tseng, Po-Yen,Hsu, Wei-Hsin,Chuang, Shih-Ching
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supporting information
p. 224 - 227
(2016/02/03)
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- Propanal Production Methods
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A product of p-tert-butylphenyl propionaldehyde and m-tert-butylphenyl propionaldehyde, wherein m-tert-butylphenyl propionaldehyde is in an amount from 6% to 60% of the combination of p-tert-butylphenyl propionaldehyde and m-tert-butylphenyl propionaldehyde. Also a method including; adding dropwise an aldehyde solution to a basic solution; and, collecting a fraction of p-tert-butyl cinnamic aldehyde m-tert-butyl cinnamic aldehyde therefrom; and, adding a transition metal catalyst to a solution of the p-tert-butyl cinnamic aldehyde in ethanol, and, collecting therefrom by distillation a product of p-tert-butylphenyl propionaldehyde and the meta isomer m-tert-butylphenyl propionaldehyde; wherein the product comprises m-tert-butylphenyl propionaldehyde in an amount from 6% to 60% of the combination of p-tert-butylphenyl propionaldehyde and m-tert-butylphenyl propionaldehyde.
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Page/Page column 3
(2010/10/19)
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