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9,9-bis[4-(2-hydroxyethoxy) phenyl] fluorene crystal polymorph and synthetic process thereof

A technology of hydroxyethoxy and synthesis process, applied in the field of 9,9-bis[4-phenyl]fluorene crystal polymorph and its synthesis process

Inactive Publication Date: 2013-10-30
JIANGSU EVER GALAXY CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As early as the 1930s and 1950s, foreign countries have studied the application of fluorenone in fuels, medicines, pesticides, plastics and functional polymer materials. In my country, there were only reagent products in the 1970s, and no large-scale production industry has yet been formed.

Method used

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  • 9,9-bis[4-(2-hydroxyethoxy) phenyl] fluorene crystal polymorph and synthetic process thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Put 36g (0.2mol) of 9-fluorenone, 165.6g (1.2mol) of ethylene glycol phenyl ether and 1mL of 3-mercapto into a 1L four-necked flask with cooling water pipe, stirring, constant pressure dropping funnel, and thermometer For propionic acid, stir and raise the temperature to 20°C, start to add 30g of concentrated sulfuric acid dropwise, and keep the temperature at 60~70°C for 12h after the dropwise addition. Add 100 g of water and 240 g of toluene at the end of the heat preservation, heat up to 80° C., separate the water phase, and wash the organic phase with water, sodium carbonate aqueous solution, and water respectively. Toluene and excess phenoxyethanol were recovered by concentrating the organic phase under reduced pressure. Add 400g of methanol to the obtained mixed solution, heat up and reflux for recrystallization, cool down to 5 degrees and filter to obtain a white 9,9-bis[4-(2-hydroxyethoxy)phenyl]fluorene crude product, and then dissolve and clarify it with ...

Embodiment 2

[0023] Put 36g (0.2mol) of 9-fluorenone, 110.4g (0.8mol) of ethylene glycol phenyl ether and 1mL of 3-mercapto into a 1L four-necked flask with cooling water pipe, stirring, constant pressure dropping funnel, and thermometer For propionic acid, stir and heat up to 20°C, start to add 30g of concentrated sulfuric acid dropwise, and keep the temperature below 70°C for 10h after the dropwise addition. Add 100 g of water and 240 g of toluene at the end of the heat preservation, heat up to 80° C., separate the water phase, and wash the organic phase with water, sodium carbonate aqueous solution, and water respectively. Toluene and excess phenoxyethanol were recovered by concentrating the organic phase under reduced pressure. Add 400g of methanol to the obtained mixed solution and heat up to reflux, cool down to 5 degrees and filter to obtain a white 9,9-bis[4-(2-hydroxyethoxy)phenyl]fluorene crude product, which is then dissolved and clarified with 200g of ethyl acetate Add...

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Abstract

The invention discloses a synthesizing process for fluorenone derivatives. In the presence of concentrated sulfuric acid and a 3-mercaptoacetic acid catalyst, 9-fluorenone and ethylene glycol phenyl ether react at certain temperature, are washed and recrystallized to prepare 9,9-bi[(4-(2- hydroxy ethoxy) phenyl] fluorene, the purity of the product is larger than 97%, the melting point of the product ranges from 106 DEG C to 161 DEG C, a low-melting-point portion accounts for 85% at least, and the volume density of the product is larger than 0.5g / cm<3>. The 9,9-bi[(4-(2- hydroxy ethoxy) phenyl] fluorene synthesized by the process has the advantages of low melting point, high stacking density, good fluidity, convenience in operation and easiness in implementation, and is favorable for popularization and application.

Description

technical field [0001] The invention relates to a 9,9-bis[4-(2-hydroxyethoxy)phenyl]fluorene crystal polymorph and a synthesis process thereof. Background technique [0002] Fluorenone is an important raw material for organic synthesis. It can be used to synthesize anticancer drugs, sympathetic nerve inhibitors and antispasmodics in the pharmaceutical industry; it can be used to synthesize herbicides and insecticides in agriculture; it can be used in the fuel industry. It can be used as a synthetic aromatic diamine fuel; it can be used to make photosensitive materials in the electrostatic copying industry; in the plastics industry, fluorenone can be used to synthesize bisphenol products, used as a stabilizer and plasticizer in the polymerization process, and to prepare functional polymer materials. As early as the 1930s and 1950s, foreign countries had researched on the application of fluorenone in fuels, medicines, pesticides, plastics and functional polymer materials. In m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/23C07C41/30
Inventor 陈东辉赵金龙
Owner JIANGSU EVER GALAXY CHEM CO LTD