- Synthesis of fluorenebisphenoxy derivatives by acid-sulfur compound catalyzed condensation reaction
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An efficient method for the synthesis of fluorenebisphenoxy derivatives from fluorenone and phenoxy compounds is successfully performed by the combined use of concentrated sulfuric acid as catalyst and 3-mercaptopropionic acid as co-catalyst. Several fluorenebisphenoxy derivatives are obtained in good yields by this one-step reaction.
- Yamada, Mitsuaki,Sun, Jun,Suda, Yasuhiro,Nakaya, Tadao
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- Efficient microwave-assisted synthesis of 9,9-bis[4-(2-hydroxyethoxy) phenyl]fluorene from 9-fluorenone and 2-phenoxyethanol
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9-Fluorenone (1) smoothly reacts with phenoxyethanol (2) in the presence of Al3+-montmorillonite catalyst and 3-mercaptopropionic acid as a cocatalyst under microwave irradiation at 160°C for 10 min to give 9,9-bis[4-(2- hydroxyethoxy)phenyl]fluorene (3) in 81% yield, which was much higher than the yield of 33% obtained by conventional heating using an oil bath. A similar acceleration effect of microwave irradiation was observed in other metal-cation-exchanged montmorillonite catalysts as well. Copyright Taylor & Francis Group, LLC.
- Hiroki, Kazuaki,Morii, Nahoko,Yamashita, Hiroshi,Sugiyama, Jun-Ichi
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- Synthesis method of 9, 9-di [4-(2-hydroxyethoxy) phenyl] fluorene
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The invention discloses a synthesis method of 9, 9di [4 -(2-hydroxy ethoxy) phenyl] fluorene, and belongs to the technical field of chemical synthesis. 9-fluorenone, phenoxyethanol, a catalyst and a cocatalyst are stirred and heated to reflux in an alkane solvent, generated water is removed from a reaction solution in an azeotropic manner while reaction is performed, water is added for dilution after the reaction is finished, the mixture is stirred uniformly, cooled, crystallized and filtered, a filter cake is rinsed and dried, and a 9, 9-di [4- (2-hydroxy ethoxy) phenyl] fluorene finished product is obtained; standing and layering the crystallized mother liquor obtained by filtering, removing a water phase, distilling an organic phase to recover the alkane solvent, and rectifying a concentrate to recover phenoxyethanol. The method has the advantages of cheap and easily available raw materials, simple operation, good atom economy, high synthesis yield, good product quality, environmental friendliness and the like, and is suitable for industrial application.
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Paragraph 0036-0060
(2021/01/15)
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- A fluorene skeleton fragrant ether class compound preparation method (by machine translation)
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A fluorene skeleton fragrant ether class compound preparation method, the difference lies in that, in order to replace the 9 - fluorenylmethylchloroformate ketone derivatives and substituted aryl ethers or substituted aryloxy alcohol compound as a raw material, in the load SO4 2 - Composite solid super strong acid catalyst catalytic reaction under the fragrant ether class containing fluorene skeleton of the compound in the crude product, obtained after purifying the product containing fluorene skeleton fragrant ether class compounds. This invention has used the composite solid super strong acid catalyst, to replace the existing process for use in the catalyst, its advantages that not only the catalyst and reaction recovery solution can be repeatedly used, the production cost is reduced, thereby improving the production efficiency, and reducing the pollution of the environment; and the reaction yield is high, the operation is simple, the product is easy to purify, is more suitable for sustainable industrial production development. (by machine translation)
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Paragraph 0031-0040; 0049-0052
(2018/12/13)
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- 9,9-BIS(4-(2-HYDROXYETHOXY)PHENYL)FLUORENE CRYSTAL
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PROBLEM TO BE SOLVED: To produce 9,9-bis(4-(2-hydroxyethoxy)phenyl)fluorene crystal which shows a melting peak by a differential scan calorimetry in a temperature region of 115-125°C and has a bulk density of 0.60-0.75 g/cm3. SOLUTION: Fluorenone and phenoxy ethanol are reacted to obtain rough crystal of 9,9-bis(4-(2-hydroxyethoxy)phenyl)fluorene, and the rough crystal is purified to prepare purified crystal of 9,9-bis(4-(2-hydroxyethoxy)phenyl)fluorene having the enhanced degree of purity to at least 99%. The purified crystal is dissolved in a mixed solvent of acetonitrile and methanol of which a temperature is controlled to -20°C to 5°C to prepare a solution, and crystal is precipitated in the solution. When the precipitated crystal is separated and dried, the target 9,9-bis(4-(2-hydroxyethoxy)phenyl)fluorene crystal is obtained. SELECTED DRAWING: None COPYRIGHT: (C)2018,JPOandINPIT
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Paragraph 0056; 0077; 0084
(2018/04/21)
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- 9, 9 - bis (4 - (2 - hydroxyethoxy) phenyl) fluorene in production, and the crystal, and production of the crystal
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A method for producing 9,9-bis(4-(2-hydroxyethoxy)phenyl)fluorene, which can be used for obtaining 9,9-bis(4-(2-hydroxyethoxy)phenyl)fluorene having a high static bulk density and a low melting point, and is characterized in that 9-fluorenone is reacted with 2-phenoxy ethanol in the presence of methanesulfonic acid and the resultant product is purified using butanol.
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Paragraph 0024
(2017/07/13)
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- 9, 9 - bis (4 - (2 - hydroxyethoxy) phenyl) fluorene crystal
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[Problem] differential scanning calorimetry melting peak is observed in the temperature range of 115 d 125 °C, and, the bulk specific gravity of 0.60-to 0.75 g/cm3 9, 9 - bis (4 - (2 - hydroxyethoxy) phenyl) fluorene in new production method of crystals. 9, 9 - bis [a] (4 - (2 - hydroxyethoxy) phenyl) fluorene in the reaction phenoxyethanol yielded crude fluorene, 9, 9 - bis at least 99% purity of the purified crude crystal (4 - (2 - hydroxyethoxy) phenyl) can be enhanced by preparation of crystals of fluorene. Methanol mixed solvent refined crystal controlled temperature - 20 c 5 °C acetonitrile solution was prepared by dissolving, in this solution to precipitate crystals, separating and drying the deposited crystals, 9, 9 - bis (4 - (2 - hydroxyethoxy) phenyl) fluorene crystal method. Figure 2 [drawing]
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Paragraph 0056
(2017/11/04)
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- 9, 9 - Bis (hydroxy alkoxy phenyl) preparation of fluorene
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For the purpose of providing a method for producing a 9,9-bis(hydroxyalkoxyphenyl)fluorene, the present invention provides a method for producing a 9,9-bis(hydroxyalkoxyphenyl)fluorene represented by general formula (3), which is characterized by reacting a 9,9-dihalogenated fluorene represented by general formula (1) with a phenoxy alcohol represented by general formula (2). (In general formula (1), each R1 independently represents an alkyl group, an alkoxy group, an aromatic hydrocarbon group or a halogen atom; X represents a halogen atom; and each m independently represents 0 or an integer of 1-4, provided that in cases where m is 2 or more, the R1 moieties may be the same as or different from each other.) (In general formula (2), R2 represents an alkyl group, an alkoxy group, an aromatic hydrocarbon group or a halogen atom; R3 represents a linear or branched alkylene group; and n represents 0 or an integer of 1-4, provided that in cases where n is 2 or more, the R2 moieties may be the same as or different from each other.) (In general formula (3), R1, R2, R3, m and n are as defined above.)
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Paragraph 0029
(2018/03/02)
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- HIGH REFRACTIVE MONOMER, RESIN COMPOSITION FOR PRISM SHEET CONTAINING THE SAME AND PRISM SHEET USING THE SAME
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Disclosed are a high refractive monomer having at least one acryl functional group in a terminal and designed to meet a refractive index more than 1.57, a resin composition for forming the prism sheet capable of controlling refraction, viscosity, hardness, and yellowness by containing the high refractive monomer only or a mixture comprising the same, a prism sheet embodying high refraction and low viscosity of a liquid before curing and having excellent clarity and yellowing resistance by using the resin composition for forming the prism sheet which is made of the optimum mix. According to the present invention, the high luminance prism sheet is provided, thereby reducing the number of the sheet applied to embody the same luminance so as to contribute to slimming down the sheet, enhancing the performance, and saving costs. Therefore, the number of LED lamps used for a backlight unit can be reduced, thereby saving energy.
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- HIGH REFRACTIVE OLIGOMER, RESIN COMPOSITION FOR PRISM SHEET CONTAINING THE SAME AND PRISM SHEET USING THE SAME
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The present invention relates to a high refractive oligomer, a resin composition for molding a prism sheet containing the same, and a prism sheet using the same. The present invention provides a low viscosity and low yellowing type highly refractive oligomer, which comprises acryl functional groups on both terminus and contains at least two urethane functional groups in a molecular structure, and meets a refractive index higher than 1.61, and provides a prism sheet embodying a high refractive index and low viscosity of a liquid before curing and having excellent transparence and yellowing resistance, and meeting excellent adhesive strength and pencil hardness after curing through the resin composition for molding the prism sheet containing the highly refractive oligomer or an optimized mixing ratio between the highly refractive oligomer and highly refractive monomer. Accordingly, the prism sheet of the present invention contributes to slimming of the sheet, performance improvement, and reduction of manufacturing costs by reducing the number of the sheets applied to embody equal luminance, thereby reducing the number of LED lamps used for a backlight unit and saving energy.
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- Method for preparing 9, 9-bis(4-(2-hydroxyethoxy)phenyl)fluorene from ethylene oxide
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The invention relates to the technical field of 9, 9-bis(4-(2-hydroxyethoxy)phenyl)fluorene synthesis and especially relates to a method for preparing 9, 9-bis(4-(2-hydroxyethoxy)phenyl)fluorene from ethylene oxide. The method comprises that in the presence of a base, at a temperature of 30-80 DEG C, ethylene oxide and 9, 9-bis(4-hydroxyphenyl)fluorene undergo a reaction according to a mass ratio of 0.25: 1 to 0.35: 1 in a polar organic solvent. The preparation method adopts ethylene oxide and 9, 9-bis(4-hydroxyphenyl)fluorene as raw materials and a base as catalyst, and the reaction occurs at the normal temperature under the normal pressure so that a raw material cost is low. The preparation method does not produce waste gas and waste residues and has small pollution on the environment. The preparation method has the advantages of simple processes and low cost and is suitable for industrial production.
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Paragraph 0025
(2017/07/01)
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- A 9,9-bis [(4-hydroxy-ethoxy) phenyl] fluorene preparation method
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The invention discloses a method for preparing 9,9-bis[(4-hydroxy oxyethyl) phenyl] fluorene and belongs to the technical field of chemical synthesis. The method is characterized by comprising the following steps: reacting 9-fluorenone and ethylene glycol monophenyl ether in hydrogen fluoride in the presence of a promoter to obtain 9,9-bis[(4-hydroxy oxyethyl) phenyl] fluorene; at the end of the reaction, evaporating to reclaim hydrogen fluoride from the reaction system, diluting residues with alkaline liquid; extracting, washing and re-crystallizing to obtain 9,9-bis[(4-hydroxy oxyethyl) phenyl] fluorene. The method has the advantages of use of low-price and easily available raw materials, high reaction yield, convenience in acid catalyst reclamation, generation of less 'three waste', environmental friendliness and the like, and has a high industrial application value.
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Paragraph 0035; 0036
(2017/02/28)
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- METHOD FOR PRODUCING FLUORENE DERIVATIVE
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A method for producing a fluorene derivative by reacting fluorenone with a phenol or a phenoxyalcohol in the presence of an acid catalyst includes: adding an alkali to an obtained reaction liquid containing a fluorene derivative; and concentrating a resultant mixture liquid without removing the alkali thus added and a reaction product of the alkali, thereby separating an unreacted phenol or unreacted phenoxyalcohol.
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Page/Page column 15
(2012/02/06)
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- CRYSTALLINE POLYMORPH OF FLUORENE DERIVATIVE AND PROCESS FOR PRODUCTION THEREOF
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A method of producing a crystal polymorph of 9,9-bis(4-(2-hydroxyethoxy)phenyl)fluorene, comprising the steps of reacting fluorenone and 2-phenoxyethanol in the presence of a heteropolyacid, initiating deposition of 9,9-bis(4-(2-hydroxyethoxy)phenyl)fluorene at lower than 50°C from the resultant mixture to obtain a crude product of 9,9-bis(4-(2-hydroxyethoxy)phenyl)fluorene, dissolving the crude product in at least one solvent selected from the group consisting of aromatic hydrocarbon solvents, ketone solvents and ester solvents, and initiating deposition of 9,9-bis(4-(2-hydroxyethoxy)phenyl)fluorene at 50°C or higher.
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Page/Page column 6
(2009/12/07)
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- Aromatic ethers and process for producing aromatic ethers
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According to a production process, aromatic ethers are producible by reacting phenols with an oxirane compound with use of an anion exchange resin as a catalyst. According to another production process, aromatic ethers having an alcoholic hydroxyl group are producible by a crystallization-purification step of using a solvent having a solubility parameter ranging from 7.5 to 12.5 for purification by crystallization. Further, according to still another production process, producible are aromatic ethers having an alcoholic hydroxyl group, wherein the content of a metal in the aromatic ethers is less than 100 ppm by mass, and the content of a halogen element in the aromatic ethers is less than 100 ppm by mass.
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- Method of preparing a fluorene derivative and the method of purifying thereof
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A fluorene derivative of high purity is produced by reacting fluorenone with phenoxyethanol in the presence of a sulfuric acid-thiol catalyst system, dissolving the reaction mixture in a lower aliphatic alcohol and adding water to the resulting solution for precipitation of 9,9-bis(4-(2-hydroxyethoxy)phenyl)fluorene [fluorene derivative]. A fluorene derivative of still higher purity is obtained by recrystallization from a lower aliphatic alcohol. In accordance with this invention, a fluorene derivative can be produced advantageously on a commercial scale without incurring any appreciable loss of fluorenone, in good yield, with high efficiency and in a reduced production time.
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