Preparation method of high-bulk density 9,9-di[3-phenyl-4-(2-hydroxyethoxy)phenyl]fluorene crystals

A hydroxyethoxy, bulk density technology, applied in ether preparation, ether separation/purification, organic chemistry and other directions, can solve the problems of unreported product melting point, bulk density and crystal form, achieve easy transfer and feeding, good use effect , the effect of high bulk density

Inactive Publication Date: 2016-12-21
JIANGSU EVER GALAXY CHEM CO LTD
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  • Abstract
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  • Application Information

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Problems solved by technology

The Japanese patent does not report the melting point, bulk density and crystal form of the product

Method used

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  • Preparation method of high-bulk density 9,9-di[3-phenyl-4-(2-hydroxyethoxy)phenyl]fluorene crystals
  • Preparation method of high-bulk density 9,9-di[3-phenyl-4-(2-hydroxyethoxy)phenyl]fluorene crystals
  • Preparation method of high-bulk density 9,9-di[3-phenyl-4-(2-hydroxyethoxy)phenyl]fluorene crystals

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Embodiment （1）

[0030] Embodiment (1) (preparation of crystalline polymorph A)

[0031] Add 9-fluorenone (18 g, 0.1 mol), 2-[(2-phenyl)phenoxy]ethanol (53.5 g, 0.25 mol), 3-mercaptopropionic acid (1 g), toluene into the reaction flask 60 mL, stirred until 9-fluorenone and 2-[(2-phenyl)phenoxy]ethanol were dissolved, then slowly added 25 mL of 98% sulfuric acid dropwise. The reaction was stirred at 65°C for 6 hours. HPLC analysis confirmed that the 9-fluorenone content was below 0.5% and the reaction was stopped. Add sodium hydroxide solution to neutralize, add water to wash until neutral, and slowly lower the temperature of the organic phase. The crude product of 9,9-bis[3-phenyl-4-(2-hydroxyethoxy)phenyl]fluorene was obtained by filtration.

[0032] The crude product was recrystallized from toluene to obtain 9,9-bis[3-phenyl-4-(2-hydroxyethoxy)phenyl]fluorene as white crystal A, which was dried under vacuum at 80°C for 20 hours to obtain 52 g, yielding The yield is 88.0%, and the purity ...

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Abstract

High-bulk density 9,9-di[3-phenyl-4-(2-hydroxyethoxy)phenyl]fluorene crystals are synthesized from 9-fluorenone and 2-[(2-phenyl)phenoxyl]ethanol in a benzene solvent with sulfuric acid as a catalyst and 3-mercaptopropionic acid as a cocatalyst, the purity (HPLC analysis) of the crystals is greater than 98%, the bulk density of the crystals is greater than 0.4g/cm<3>, and the crystals have good fluidity. The endothermic melting peak range of the crystals is 142-180 DEG C. An X-powder diffraction (XRPD) analysis result shows that the characteristic 2theta values of the crystals are 7.60(47), 15.60(57), 16.40(55), 17.20(48), 18.70(49), 19.00(67), 20.60(100), 21.50(38) and 23.7(40).

Description

technical field [0001] The present invention relates to the high packing density of 9,9-bis[3-phenyl-4-(2-hydroxyethoxy)phenyl]fluorene and the preparation of novel crystal polymorphs. Background technique [0002] 9,9-bis[3-phenyl-4-(2-hydroxyethoxy)phenyl]fluorene is an important intermediate of photoelectric materials, and the epoxy resin and acrylic resin derived from it have high refractive index, thermal Excellent properties such as high stability and good transparency have important applications in light-emitting diode packaging materials, light guide devices, enhancement films, polarizing films, reflective films, optical lenses, gas separation films, and electronic lithography materials. [0003] Japanese patents JP5285561B, JP2011074222A and JP5325627B have reported the preparation method of 9,9-bis[3-phenyl-4-(2-hydroxyethoxy)phenyl]fluorene (the preparation method steps of the three patents are the same), and the concentrated Sulfuric acid is used as a catalyst, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/23C07C41/40
CPCC07C41/40C07B2200/13C07C43/23
Inventor 田礼彬陆国元张强
Owner JIANGSU EVER GALAXY CHEM CO LTD
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