156570-10-4Relevant articles and documents
Synthesis method of diethyl 2-[2-(2,4-difluorophenyl)allyl]-1,3-malonate
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Paragraph 0016; 0034; 0036, (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.
Synthesis method of 2-[2-(2,4-diflurophenyl)-2-propylene-1-yl]-1,3-propylene glycol
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Paragraph 0038, (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.
Synthesis method of 2-[2-(2,4-diflurophenyl)propenyl]-1,3-diethyl malonate
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Paragraph 0038, (2017/04/19)
The invention relates to a synthesis method of 2-[2-(2,4-diflurophenyl)propenyl]-1,3-diethyl malonate. The synthesis method of 2-[2-(2,4-diflurophenyl)propenyl]-1,3-diethyl malonate is characterized in that the synthesis method comprises the following steps: (1) 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; (2) mixing 2-(2,4-diflurophenyl)-1-chloro-3-propanol obtained in step (1) with potassium hydrogen sulfate and chlorobenzene to perform reaction to obtain 1-(1-chloromethylvinyl)-2,4-difluorobenzene; (3) enabling 1-(1-chloromethylvinyl)-2,4-difluorobenzene obtained in step (2) to react with diethyl malonate to obtain a target product 2-[2-(2,4-diflurophenyl)propenyl]-1,3-diethyl malonate; a specific synthesis route is as shown in the accompanying drawing.