1254177-54-2Relevant articles and documents
Double-substituted nitrobenzene acetonitrile derivative of the solvent-free preparation method
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Paragraph 0018; 0020-0025; 0031-0036; 0059-0061, (2019/05/11)
Double-substituted nitrobenzene acetonitrile derivative of the solvent-free preparation method, comprises the following steps: a, will be to the nitrobenzene acetonitrile, aromatic aldehyde, alkali and dihydro pyridine ester in accordance with the molar ratio of 1: (1 - 2): (0.2 - 1.5): (1 - 2) are added to a reaction in the test tube, heating up to 80 - 100 °C, stirring 0.5 - 12 h Knoevenagel condensation - reduction in series on the reaction; b, the product obtained in step a, in accordance with to the nitrobenzene with an alkali, to [...] 1: (1 - 4): (1 - 4) of adding alkali and [...] molar ratio, heating up to 80 - 100 °C, stirring 0.5 - 3 h carrying out the alkylation reaction; (3) the step b of the obtained product is carried out column chromatography, the final double-substituted nitrobenzene acetonitrile derivative products. This invention does not need to use a solvent for preparing double-substituted nitrobenzene acetonitrile product, solves the technical need to use the solvent not economic the issue of environmental protection, in addition, also has simplified the reaction step, improving the existing synthetic reaction time is long.
Solvent-free 2-p-nitrophenyl-3-aryl propionitrile and preparation method thereof
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Paragraph 0034-0048, (2018/04/01)
The invention discloses a solvent-free 2-p-nitrophenyl-3-aryl propionitrile and a preparation method thereof. The preparation method comprises the following steps: adding 4-nitrophenylacetonitrile, aromatic aldehyde, alkali and dihydropyridine ester into a reaction test tube and performing stirring reaction; performing column chromatography to obtain the product 2-p-nitrophenyl-3-aryl propionitrile, wherein the stationary phase used according to the column chromatography is a silica gel column. The problems that the solvent in the prior art is not economic and is not environmentally friendly and the reaction time is long are solved, and the technical gap that the 2-p-nitrophenyl-3-aryl propionitrile is prepared by taking the dihydropyridine ester as a hydrogen source under the solvent-free condition is remedied; by a one-pot method, Knoevenagel and reduction two-step reaction are connected in series, the reaction steps are simplified, and a target product can be obtained efficiently. The dihydropyridine ester serves as the hydrogen source, so compared with the traditional hydrogen source, the hydrogen source has the advantages of no toxicity, mild reaction condition and high chemical selectivity.
Base-Promoted Cascade Approach for the Preparation of Reduced Knoevenagel Adducts Using Hantzsch Esters as Reducing Agent in Water
He, Tao,Shi, Ronghua,Gong, Yimou,Jiang, Guangyou,Liu, Ming,Qian, Shan,Wang, Zhouyu
supporting information, p. 1864 - 1869 (2016/07/16)
A cascade Knoevenagel condensation-reduction approach, which was carried out in water, has been reported. Using Hantzsch esters as reducing agent, under the promotion of base, a variety of reduced Knoevenagel adducts could be easily prepared by direct alkylation of malononitrile, ethyl 2-cyanoacetate, and 2-(4-nitrophenyl)acetonitrile, respectively. Meanwhile, a gram-scale synthesis of the protocol was also realized with excellent isolated yield.