165115-73-1Relevant articles and documents
Iron-catalyzed regiodivergent alkyne hydrosilylation
Hu, Meng-Yang,He, Peng,Qiao, Tian-Zhang,Sun, Wei,Li, Wen-Tao,Lian, Jie,Li, Jin-Hong,Zhu, Shou-Fei
, p. 16894 - 16902 (2020/10/09)
Although tremendous effort has been devoted to the development of methods for iron catalysis, few of the catalysts reported to date exhibit clear superiority to other metal catalysts, and the mechanisms of most iron catalysis remain unclear. Herein, we report that iron complexes bearing 2,9-diaryl-1,10-phenanthroline ligands exhibit not only unprecedented catalytic activity but also unusual ligand-controlled divergent regioselectivity in hydrosilylation reactions of various alkynes. The hydrosilylation protocol described herein provides a highly efficient method for preparing useful di- and trisubstituted olefins on a relatively large scale under mild conditions, and its use markedly improved the synthetic efficiency of a number of bioactive compounds. Mechanistic studies based on control experiments and density functional theory calculations were performed to understand the catalytic pathway and the observed regioselectivity.
Method for synthesizing 2-[2-(2,4-difluorophenyl)-2-propylene-1-yl]-1,3-propylene glycol
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, (2017/03/24)
The invention discloses a method for synthesizing 2-[2-(2,4-difluorophenyl)-2-propylene-1-yl]-1,3-propylene glycol. The method comprises the following steps: dropwise adding 1,2,3-trichloropropane into 1,3-difluorobenzene; 20-40min later, adding aluminium trichloride; keeping reactions for 0.5-1.5h at 5-(-5) DEG C; heating to 20-45 DEG C and keeping reactions for 1.5-3h; adding the product into a hydrochloric acid solution and extracting; washing once using saturated NaHCO3 solution, water and saturated saline solution in sequence; drying with anhydrous Na2SO4 and filtering; evaporating to remove the solvent to obtain 1,3-dichloro-2-(2,4-difluorophenyl)propane; adding 1,3-dichloro-2-(2,4-difluorophenyl)propane and potassium hydroxide into tert-butyl alcohol, and enabling backflow for 3.5-6h; removing the tert-butyl alcohol; adding ice water and neutralizing to neutrality using hydrochloric acid at 5-(-5) DEG C; extracting using dichloromethane for three times; drying using anhydrous Na2SO4 and filtering; dissolving the evaporation and distillation product in DMSO, and adding diethyl malonate and hydroxide for reactions; and enabling the obtained product to react with lithium chloride and sodium borohydride to obtain a target product, wherein the synthesis path is shown in the specification.
Synthesis method of 2-[2-(2,4-diflurophenyl)-2-propylene-1-yl]-1,3-propylene glycol
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, (2017/04/03)
The invention relates to a synthesis method of 2-[2-(2,4-diflurophenyl)-2-propylene-1-yl]-1,3-propyl glycol. The synthesis method comprises the following steps: mixing 3-chloro-1,2-propyl glycol with 1,3-difluorphenyl, adding a catalyst, reacting for 6-10 hours at room temperature, heating to 50-70 DEG C, and reacting for 2-4 hours; adding obtained mixture into hydrochloric acid solution at the temperature ranging from -5 DEG C to 5 DEG C, uniformly stirring, extracting for 3-5 times by taking dichloromethane as an extracting agent, and washing extract liquor once with saturated NaHCO3 solution, water and saturated saline solution; drying with anhydrous Na2SO4 and filtering, and evaporating dichloromethane to obtain 1-chloro-2-(2,4-diflurophenyl)-3-propyl glycol; adding 1-chloro-2-(2,4-diflurophenyl)-3-propyl glycol and potassium hydrogen sulphate into chlorobenzene, heating and refluxing for 10-16 hours; washing to be neutral, drying with anhydrous Na2SO4, then filtering, dissolving a distillation product into DMSO, adding diethyl malonate and hydroxide, reacting, and then carrying out reaction on the obtained products with lithium chloride and sodium borohydride, so that the target product is obtained, wherein a synthesis route is described in the specification.