159276-62-7Relevant articles and documents
Synthesis method of 2-[2-(2,4-diflurophenyl)-2-propen-1-yl)-1,3-propanediol
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, (2017/04/03)
The invention relates to a synthesis method of 2-[2-(2,4-diflurophenyl)-2-propen-1-yl)-1,3-propanediol. The synthesis method comprises the following steps: mixing 2-chloromethyl epoxy propane with 1,3-difluorobenzene to perform reaction under an effect of catalyst to obtain 2-(2,4-diflurophenyl)-1-chloro-3-propanol; mixing 2-(2,4-diflurophenyl)-1-chloro-3-propanol with potassium hydrogen sulfate and chlorobenzene to perform reaction to obtain 1-(1-chloromethylvinyl)-2,4-difluorobenzene; enabling 1-(1-chloromethylvinyl)-2,4-difluorobenzene to react with diethyl malonate to obtain a product 2-[2-(2,4-diflurophenyl)propenyl]-1,3-diethyl malonate; dissolving 2-[2-(2,4-diflurophenyl)-2-propen-1-yl]-1,3-diethyl malonate in mixed solvent formed by isopropanol and water to react with borohydride to obtain a target product 2-[2-(2,4-diflurophenyl)-2-propen-1-yl)-1,3-propanediol; a synthesis route is as shown in the accompanying drawing.
Method for synthesizing 2-methyl propionate-[(2S)-4-(2,4-diflurophenyl)-2-hydroxymethyl-4-amylene-1-group] ester
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, (2016/12/12)
The invention provides a method for synthesizing 2-methyl propionate-[(2S)-4-(2,4-diflurophenyl)-2-hydroxymethyl-4-amylene-1-group] ester.The method includes the steps that 1,2,3-trichloropropane is added dropwise to 1,3-difluorobenzene, and aluminum trichloride is added for a reaction; the mixture is added to a hydrochloric acid solution for extraction, and washing is conducted with a saturated NaHCO3 solution, water and saturated salt solution in sequence; anhydrous Na2SO4 is used for drying and filtering, evaporation is conducted for solvent removal, and 1,3-dichloro-2-(2,4-diflurophenyl) propane is obtained; 1,3-dichloro-2-(2,4-diflurophenyl) propane and potassium hydroxide are added to tert butyl alcohol, and reflux is conducted for 3.5-6 h; tert butyl alcohol is removed, ice water is added, the mixture is neutralized with hydrochloric acid at the temperature of 5 to -5 DEG C to be neutral, dichloromethane is used for three times of extraction, anhydrous Na2SO4 is used for drying and filtering, a distillation product is dissolved in DMSO, a product obtained after diethyl malonate and diethyl malonate react are added and a product obtained after lithium chloride and sodium borohydride react are added and dissolved in methylbenzene, and sodium bicarbonate, Novo SP 435 esterifying enzymes and isobutyric anhydride are added for a reaction; the target product is obtained after washing, crystallization and drying are conducted.The synthesis path is shown in the description.
Synthesis method of diethyl 2-[2-(2,4-difluorophenyl)allyl]-1,3-malonate
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, (2017/02/28)
The invention relates to a synthesis method of diethyl 2-[2-(2,4-difluorophenyl)allyl]-1,3-malonate. The synthesis method comprises the following steps: mixing 3-chloro-1,2-propanediol and 1,3-difluorobenzene, and adding a catalyst to react; adding the mixture into a hydrochloric acid solution at 5 to -5 DEG C, stirring uniformly, extracting 3-5 times by using dichloromethane as an extractant, and washing the extracting solution with a saturated NaHCO3 solution, water and a saturated saline solution; drying with anhydrous Na2SO4, filtering, evaporating the dichloromethane to obtain 1-chloro-2-(2,4-difluorophenyl)-3-propanol, mixing the 1-chloro-2-(2,4-difluorophenyl)-3-propanol and potassium hydrogen sulfate into chlorobenzene, and heating under reflux for 10-16 hours; and washing with water to a neutral state, drying with anhydrous Na2SO4, filtering, distilling to obtain 1-(1-chloromethylvinyl)-2,4-difluorobenzene, dissolving in DMSO (dimethyl sulfoxide), adding diethyl malonate and hydroxide to react, extracting, washing and carrying out reduced pressure distillation to obtain the target product. The synthesis route is disclosed in the specification.