87676-93-5Relevant articles and documents
Preparation of a novel bridged bis(β-cyclodextrin) chiral stationary phase by thiol-ene click chemistry for enhanced enantioseparation in HPLC
Gong, Bolin,Guo, Siyu,Zhang, Ning
, p. 35754 - 35764 (2021/12/02)
A bridged bis(β-cyclodextrin) ligand was firstly synthesized via a thiol-ene click chemistry reaction between allyl-ureido-β-cyclodextrin and 4-4′-thiobisthiophenol, which was then bonded onto a 5 μm spherical silica gel to obtain a novel bridged bis(β-cyclodextrin) chiral stationary phase (HTCDP). The structures of HTCDP and the bridged bis(β-cyclodextrin) ligand were characterized by the 1H nuclear magnetic resonance (1H NMR), solid state 13C nuclear magnetic resonance (13C NMR) spectra spectrum, scanning electron microscope, elemental analysis, mass spectrometry, infrared spectrometry and thermogravimetric analysis. The performance of HTCDP in enantioseparation was systematically examined by separating 21 chiral compounds, including 8 flavanones, 8 triazole pesticides and 5 other common chiral drugs (benzoin, praziquantel, 1-1′-bi-2-naphthol, Tr?ger's base and bicalutamide) in the reversed-phase chromatographic mode. By optimizing the chromatographic conditions such as formic acid content, mobile phase composition, pH values and column temperature, 19 analytes were completely separated with high resolution (1.50-4.48), in which the enantiomeric resolution of silymarin, 4-hydroxyflavanone, 2-hydroxyflavanone and flavanone were up to 4.34, 4.48, 3.89 and 3.06 within 35 min, respectively. Compared to the native β-CD chiral stationary phase (CDCSP), HTCDP had superior enantiomer separation and chiral recognition abilities. For example, HTCDP completely separated 5 other common chiral drugs, 2 flavanones and 3 triazole pesticides that CDCSP failed to separate. Unlike CDCSP, which has a small cavity (0.65 nm), the two cavities in HTCDP joined by the aryl connector could synergistically accommodate relatively bulky chiral analytes. Thus, HTCDP may have a broader prospect in enantiomeric separation, analysis and detection. This journal is
Continuous preparation method of flutriafol
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Paragraph 0009; 0040-0048, (2019/02/26)
The invention relates to a continuous preparation method of flutriafol. 1,2,4-triazole and 1-(2-fluorophenyl)-1-(4-fluorophenyl) ethylene oxide react in a microchannel continuous flow reactor in the presence of an organic solvent and a soluble alkali to obtain the flutriafol. The method is short in reaction time and high in automatic production level, promotes the competitiveness of an enterprise,is small in safety hazard in the process of synthesizing the target product, reduces the risk coefficient, is high in yield of the target product, simple in post treatment and little in solid waste,and realizes a cleaner and environment-friendly production process.
A synthesis method of flutriafol (by machine translation)
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Paragraph 0034; 0037; 0039-0054, (2019/01/08)
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)