- Synthesizing process of flutriafol key intermediate 1-(2-fluorophenyl)-1-(4-fluorophenyl)ethylene oxide
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The invention discloses a synthesizing process of a flutriafol key intermediate 1-(2-fluorophenyl)-1-(4-fluorophenyl)ethylene oxide. The synthesizing process comprises the following steps: mixing 1-bromooctane and sodium methyl mercaptide, adding tetrabutylammonium bromide, stirring for reacting, adding water for standing and layering to form an organic phase and a water phase after the reaction is finished, performing skimming to remove the water phase, washing the organic phase with water, performing drying and suction filtration, dissolving a prepared product and dimethyl sulfate in an organic solvent for reacting, and removing the organic solvent from a reaction solution to obtain sulfur-onium salt after the reaction is finished; adding the sulfur-onium salt, inorganic alkali and 2,4'-difluoro benzophenone into a solvent, stirring for reacting, adding water for standing and layering to form an organic phase and a water phase after the reaction is finished, performing skimming to remove the water phase, washing the organic phase with water, performing dehydration, drying and suction filtration, and removing the solvent from filtrate to obtain the 1-(2-fluorophenyl)-1-(4-fluorophenyl)ethylene oxide. By adopting the synthesizing process, the alkali is screened, and sodium hydroxide is taken as an alkali medium, thereby improving the reaction yield; moreover, methyl n-octyl sulfide has low odor.
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Paragraph 0013; 0014; 0015-0016
(2019/02/25)
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- Synthetic method of 1-(2-fluorophenyl)-1-(4-fluorophenyl)ethylene oxide
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The invention discloses a synthetic method of 1-(2-fluorophenyl)-1-(4-fluorophenyl)ethylene oxide, comprising the following steps: firstly mixing 1-bromo-n-decane and sodium methyl mercaptide, addingtetrabutylammonium bromide and carrying out a reaction, and conducting aftertreatment on the reaction product so as to obtain n-decyl methyl sulfide; dissolving n-decyl methyl sulfide and dimethyl sulfate in a solvent I, and carrying out a heating reflux reaction; carrying out reduced pressure distillation of the solvent I after the reaction so as to obtain a reaction product containing sulfoniumsalt; carrying out an epoxidation reaction by successively adding the reaction product containing sulfonium salt, sodium hydroxide and 2,4'-difluorobenzophenone into a solvent II, and carrying out aftertreatment after the reaction so as to obtain 1-(2-fluorophenyl)-1-(4-fluorophenyl)ethylene oxide. By the method for synthesizing 1-(2-fluorophenyl)-1-(4-fluorophenyl)ethylene oxide, the invention has technical advantages of environmental protection, high yield and the like.
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Paragraph 0030; 0033-0036; 0037; 0040-0043; 0047; 0052
(2019/01/21)
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- A synthesis method of flutriafol (by machine translation)
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The invention relates to a synthesis method of flutriafol, the halogenated methane and dimethyl sulfoxide in the 0 - 120 °C reaction under 1 - 48 H-; adding solid alkali and 2, 4' - difluoro benzophenone, temperature control in the 0 - 80 °C, reaction 1 - 25 the H; adding triazole, temperature control in the 50 - 200 °C, reaction 1 - 20 the H, after the reaction, filtered, to remove solvent, washing, crystallization get said teflubenzuron. In the present invention dimethyl sulfoxide is used as the reaction raw material, but also as the solvent, avoiding mixed solvent separation difficulties, and, dimethyl sulfoxide and halogenated methane to replace the existing technology to the environment in the pressure of the dimethyl sulfide and highly toxic chemicals dimethyl sulfate, so that the present invention is friendly to the environment, in addition, the invention mild reaction conditions, the reaction time is short, high yield, high product quality, three waste emissions low, produces only a sole inorganic salt, of the present invention thereby the productivity is high, economic efficiency is good. (by machine translation)
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Paragraph 0053; 0054
(2019/01/08)
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- Efficient and Enantioselective Rhodium(I)-Catalyzed Arylation of α-Ketoesters: Synthesis of (S)-Flutriafol
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An enantioselective addition of arylboronic acids and α-ketoesters promoted by a Rhodium(I)-chiral diene catalyst is reported. The transformation proceeds regioselectively in the presence of as low as 0.5 mol% of the catalyst generated in situ from a Rhod
- Chang, Chiung-An,Uang, Tsung-Ying,Jian, Jia-Hong,Zhou, Meng-Yi,Chen, Ming-Liang,Kuo, Ting-Shen,Wu, Ping-Yu,Wu, Hsyueh-Liang
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p. 3381 - 3390
(2018/08/06)
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- Stereoselective synthesis of (+)-flutriafol
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The stereoselective synthesis of (+)-flutriafol, a triazole fungicide, has been accomplished in seven linear steps from (1S)-[(4R)-2,2-dimethyl-[1,3]-dioxolan-4-yl]-(4-methoxyphenyl)methanol in 15% overall yield. Diastereoselective nucleophilic 1,2-addition was employed as a key step for constructing the requisite chiral 1,2-diol for flutriafol. A high degree of 1,4-asymmetric induction could be realized via a chelation-controlled mechanism during the key alkylation step.
- Chang, Minsun,Kim, Tae Hyun,Kim, Hee-Doo
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p. 1503 - 1507
(2008/12/21)
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