92339-07-6Relevant articles and documents
Synthesis method of 2,3,5,6-tetrafluoro-4-methoxymethyl benzyl alcohol
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Paragraph 0047-0048; 0063-0064, (2019/03/30)
The invention discloses a method for synthesizing 2,3,5,6-tetrafluoro-4-methoxymethyl benzyl alcohol through 1,4-di(methoxymethyl)-2,3,5,6-tetrafluorobenzene and belongs to the technical field of organic synthesis. The method comprises the following steps: taking the 1,4-di(methoxymethyl)-2,3,5,6-tetrafluorobenzene to react in a mixed solution composed of a sulfuric acid water solution and organiccarboxylic acid; carrying out ester group hydrolysis reaction on an obtained mixture under the action of inorganic alkali; carrying out methylation reaction of hydroxyl under the action of the inorganic alkali; finally, separating and purifying to obtain the 2,3,5,6-tetrafluoro-4-methoxymethyl benzyl alcohol and recycling the 1,4-di(methoxymethyl)-2,3,5,6-tetrafluorobenzene. According to the method provided by the invention, resource utilization of the low-value 1,4-di(methoxymethyl)-2,3,5,6-tetrafluorobenzene is realized; meanwhile, the method has the advantages of cheap and easy-to-obtain reaction reagents, moderate reaction conditions, simplicity in operation, high synthesis yield, good product quality and the like, and has very high social and economic value.
Extending the series of p-substituted tetrafluorobenzoic acids: synthesis, properties and structure
Zaitsev, Kirill V.,Oprunenko, Yuri F.,Lermontova, Elmira Kh.,Churakov, Andrei V.
, p. 49 - 58 (2017/03/22)
The synthesis of the derivatives of p-aminotetrafluorobenzoic acid, p-H2NC6F4CO2H (2b), by hydrolysis, acylation or interaction with aldehydes was developed giving H2NC6F4CO2K (2a), C6F5C(O)N(H)C6F4CO2Et (3) and (E)-ArCH[dbnd]NC6F4CO2Et (4–11). The chemical derivatization of tetrafluoroterephthalic acid, p-HO2CC6F4CO2H (12), by hydrolysis, etherification and reduction was performed giving a number of symmetrical X(O)CC6F4C(O)X (13–15; X?=?Cl, NEt2, OMe) or unsymmetrical YC6F4CO2Me (15a–b, 16, 18–21; Y?=?CO2K, CO2H, CH2OH, C(O)Cl, C(O)C6H3(i-Pr)2, CO2CH2C6F4CO2Me, CO2C6H4Bu-t), HOCH2C6F4CO2H (17), [MeO2CC6F4]2Y (22, 23; Y?=?OCH2CH2O, N(H)C6H4N(H)) compounds. All substances were thoroughly investigated by spectroscopic methods (multinuclear NMR and IR spectroscopy, mass-spectrometry). The molecular structures of p-H2NC6F4CO2Et (2) and p-HO2CC6F4CO2Me (15b) have been determined by X-ray diffraction analysis.
Preparation method of 2,3,5,6-tetrafluorohydrazine-1,4-benzene dimethanol
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Paragraph 0049; 0050, (2017/05/10)
The invention discloses a preparation method of 2,3,5,6-tetrafluorohydrazine-1,4-benzene dimethanol, and belongs to the technical field of fine chemical synthesis. The preparation method is characterized by comprising the following reaction steps that (1) chlorine is led into paraxylene under catalyzing of a catalyst and irradiation of visible light to achieve chlorination, then nitrogen is led in to expel residual hydrogen chloride gas, and 1,4-dual(trichloromethyl)-2,3,5,6-tetrachlorobenzene is obtained; (2) the 1,4-dual(trichloromethyl)-2,3,5,6-tetrachlorobenzene and potassium fluoride are subject to fluorization and alcoholysis in an alcohol solvent, the solvent is recycled through reduced pressure distillation, washing is carried out the neutral state is obtained, drying is carried out, and 1,4-dual(silane oxygen methyl chloride)-2,3,5,6-tetrachlorobenzene is obtained; and (3) hydrogen is led into the 1,4-dual(silane oxygen methyl chloride)-2,3,5,6-tetrachlorobenzene in a solvent containing a metal catalyst and an acid-binding agent to be subject to catalytic hydrogenation reduction, an upper-layer organic phase is subject to cooling, suction filtration and drying to obtain the2,3,5,6-tetrafluorohydrazine-1,4-benzene dimethanol. The preparation method has the beneficial effects that the raw materials are low in price and easy to obtain, the synthetic route is short, operation is easy and convenient, and the product cost is low.
