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Method for preparing spirofluorene derivative monomolecular resin by one-pot method

The technology of a compound and a reaction kettle is applied in the field of preparation technology for synthesizing spirofluorene derivative monomolecular resin in large quantities, and can solve the problems of complicated reaction operation process, difficulty in large-scale production of spirofluorene derivative monomolecular resin, low production efficiency, etc. , to achieve the effect of simplifying the operation steps, high reaction yield and reducing the cost of raw materials

Active Publication Date: 2021-10-26
国科天骥(山东)新材料有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this patent, the synthesis steps of spirofluorene derivative monomolecular resin are three-step reactions, and the three-step reactions are carried out separately, and the products of each step need to be separated and purified as raw materials for the next step reaction. The reaction operation process is complicated and the production efficiency is low. It has brought great difficulty to the large-scale production of spirofluorene derivative single-molecule resin

Method used

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  • Method for preparing spirofluorene derivative monomolecular resin by one-pot method

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Experimental program
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Effect test

Embodiment 1

[0039] 1) Coupling reaction

[0040] To prepare 2,7,2',7'-tetrakis-(3,4-dimethoxyphenyl)-9,9'-spirofluorene, the synthetic route is as follows:

[0041]

[0042] Add 1264g (2mol) of tetrabromospirofluorene and 1600g (8.8mol) of 3,4-dimethoxyphenylboronic acid into a 20-liter reactor, then add 4 liters of aqueous solution containing 933g (8.8mol) of sodium carbonate and 4 liters of DMF, 23 g (0.02 mol) of tetrakis(triphenylphosphine) palladium, a coupling reaction catalyst, was added in one go, and the reaction solution was heated to reflux for 10 hours. Stop heating, add 4 liters of water to the reaction system, the reaction solution is cooled to room temperature, and a large amount of granular white solid is precipitated, and the liquid (DMF and water mixture) is slowly discharged from the bottom of the reaction kettle, and the solid remains in the kettle. , add 4 liters of ethyl acetate to the reaction kettle, dissolve the solid, extract and wash the organic layer with w...

Embodiment 2

[0070] 1) Coupling reaction

[0071] To prepare 2,7,2',7'-tetrakis-(3,4,5-trimethoxyphenyl)-9,9'-spirofluorene, the synthetic route is as follows:

[0072]

[0073] Add 1264g (2mol) of tetrabromospirofluorene and 1865g (8.8mol) of 3,4,5-trimethoxyphenylboronic acid into a 20-liter reactor, and then add 6 liters of aqueous solution containing sodium hydroxide (352g, 8.8mol) and 4 liters of DMF, 69 g (0.06 mol) of tetrakis(triphenylphosphine) palladium, a coupling reaction catalyst, was added at one time, and the reaction solution was heated to reflux for 10 hours. Stop heating, add 2.5 liters of water to the reaction system, the reaction solution is cooled to room temperature, and a large amount of granular white solids are precipitated, and the liquid (DMF and water mixture) is slowly released from the bottom of the reaction kettle, and the solid remains in the kettle. , add 4 liters of ethyl acetate to the reaction kettle, dissolve the solid, extract and wash the organic la...

Embodiment 3

[0083] 1) Coupling reaction

[0084] To prepare 2,7,2',7'-tetrakis-(4-methoxyphenyl)-9,9'-spirofluorene, the synthetic route is as follows:

[0085]

[0086] Add 1264g (2mol) of tetrabromospirofluorene and 1338g (8.8mol) of 4-methoxyphenylboronic acid in a 20-liter reactor, then add 4 liters of aqueous solution containing 1214g (8.8mol) of potassium carbonate and 4 liters of DMF, once 11.5 g (0.01 mol) of tetrakis(triphenylphosphine)palladium, a coupling reaction catalyst, was added, and the reaction solution was heated to reflux for 3 hours. Stop heating, add 4 liters of water to the reaction system, the reaction solution is cooled to room temperature, and a large amount of granular white solids are precipitated, and the liquid (DMF and water mixture) is slowly released from the bottom of the reaction kettle, and the solids are left in the kettle. , add 4 liters of ethyl acetate to the reaction kettle, dissolve the solid, extract and wash the organic layer with water unti...

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Abstract

The invention relates to a method for synthesizing spirofluorene derivative monomolecular resin by one-pot method. The method of the present invention greatly simplifies the operation steps in the preparation process, and the whole operation process is carried out continuously in one reactor, which reduces the equipment cost and raw material cost, and the reaction yield is very high at the same time, and the total yield of the product can reach 90% More than %, it is suitable for industrialized large-scale production.

Description

technical field [0001] The invention belongs to the field of pilot-scale synthesis technology of photoresist materials, and specifically discloses a preparation technology for large-scale synthesis of spirofluorene derivative monomolecular resin by using a one-pot method. Background technique [0002] Photoresist is a kind of etching-resistant thin film material whose solubility changes after energy radiation such as beam, electron beam, ion beam or x-ray, and is widely used in the microfabrication of integrated circuits and semiconductor discrete devices. By coating the photoresist on the surface of a semiconductor, conductor or insulator, the part left after exposure and development will protect the bottom layer, and then use an etchant to etch to transfer the required fine pattern from the mask to the substrate. Therefore, photoresist is a key material in device microfabrication technology. Traditional photoresist host materials use polymer resins with a molecular weight...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C41/30C07C43/21C07C37/055C07C39/17C07C68/00C07C69/96
CPCC07C37/055C07C41/30C07C68/00C07C43/21C07C39/17C07C69/96
Inventor 陈金平李嫕于天君曾毅
Owner 国科天骥(山东)新材料有限责任公司