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Preparing process of tri (4-ethoxy phenyl) bismuth

A technology of ethoxyphenyl and phenetole, which is applied in the direction of bismuth organic compounds, can solve the problems of long reaction time, poor safety, and high cost, and achieve the effects of short reaction time, increased yield, and good product quality

Inactive Publication Date: 2007-06-27
SHANGHAI CHEM REAGENT RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem solved by the present invention is to provide a preparation method of tris(4-ethoxyphenyl)bismuth, to overcome the disadvantages of poor safety, long reaction time, low yield and high cost in the prior art

Method used

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  • Preparing process of tri (4-ethoxy phenyl) bismuth
  • Preparing process of tri (4-ethoxy phenyl) bismuth

Examples

Experimental program
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Effect test

Embodiment 1

[0025] In a 500ml four-neck flask equipped with heating, stirring, thermometer, reflux condenser, and drying tube, add 0.45mol (10.8g) magnesium powder, 20ml tetrahydrofuran (THF), 0.3g bromoethane, introduce nitrogen, and nitrogen atmosphere Under stirring, 0.05g iodine was added to initiate the reaction, and a mixture of 0.4mol (62.7g) 4-chlorophenetole and 50ml THF was slowly added dropwise within 1.5 hours, heated to reflux, and reacted for 5 hours. Cool to room temperature, add dropwise a mixture of 0.13mol (41.2g) bismuth trichloride and 120ml THF within 1 hour, heat up to reflux, react for 3 hours, cool to room temperature, and pour the reaction solution into 200ml of 15% hydrochloric acid solution. Add 100ml of benzene for extraction, wash the separated organic phase with water until neutral, dry over anhydrous sodium sulfate, filter, evaporate the filtrate to remove the solvent, and obtain the crude product of tris(4-ethoxyphenyl)bismuth, mix it with 550ml of benzene / e...

Embodiment 2

[0027] Add respectively 0.416mol (10g) magnesium powder, 20ml tetrahydrofuran (THF), 0.5g bromopropane in a 500ml four-necked flask with a thermometer, a reflux condenser, and a drying tube, introduce nitrogen, and stir under a nitrogen atmosphere. 0.1 g of liquid bromine was added to initiate the reaction, and a mixture of 0.4 mol (80.4 g) of 4-bromophenetole and 100 ml of THF was slowly added dropwise within 1 hour, heated to reflux, and reacted for 3 hours. Cool to room temperature, drop in 0.12mol (38g) bismuth trichloride and 100ml THF mixed solution within 40 minutes, heat up to reflux, react for 2.5 hours, cool to room temperature, pour the reaction solution into 200ml 20% sulfuric acid solution, add 100ml of benzene is extracted, and the separated organic phase is washed with water to neutrality, dried over anhydrous sodium sulfate, filtered, and the filtrate is evaporated to remove the solvent to obtain the crude product of tris(4-ethoxyphenyl)bismuth, which is washed ...

Embodiment 3

[0029] Add 0.41mol (9.8g) of magnesium powder, 20ml of tetrahydrofuran (THF), and 0.4g of bromoethane into a 500ml four-necked flask equipped with heating, stirring, thermometer, reflux condenser, and drying tube, introduce nitrogen, and Stir, add 0.05g of iodine to initiate the reaction, slowly drop in a mixture of 0.4mol (80.4g) 4-bromophenetole and 120ml THF within 1.5 hours, heat up to reflux, and react for 4.5 hours. Cool to room temperature, add dropwise the mixed solution of 0.13mol (41.2g) bismuth trichloride and 120ml THF within 40 minutes, heat up to reflux, react for 1.5 hours, cool to room temperature, and pour the reaction solution into 200ml 20% sulfuric acid solution, Add 150ml of benzene for extraction, the separated organic phase is washed with water to neutrality, dried over anhydrous sodium sulfate, filtered, and the filtrate is evaporated to remove the solvent to obtain the crude product of tris(4-ethoxyphenyl)bismuth, which is mixed with 600ml of benzene / et...

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Abstract

The present invention discloses preparation process of tri (4-ethoxy phenyl) bismuth. The present invention prepares tri (4-ethoxy phenyl) bismuth with 4-halogeno phenetole as main material, and through reaction with Grignard reagent, which is produced through reaction of alkyl halide, magnesium powder and tetrahydrofuran, and the tetrahydrofuran solution of bismuth trichloride in tetrahydrofuran as reaction solvent. The process of the present invention can obtain tri (4-ethoxy phenyl) bismuth with purity over 99 % and smelting point of 72.4-74.1 deg.c in yield of 80-85 %. Compared with available technology, the present invention has the advantages of mild reaction condition, short reaction period, high product quality, etc and is suitable for industrial production.

Description

technical field [0001] The invention relates to an improvement of a preparation method of tris(4-ethoxyphenyl)bismuth. Background technique [0002] Tris(4-ethoxyphenyl)bismuth is an important curing catalyst for polymer materials, especially widely used in polyurethane materials. Its structural formula is as follows: [0003] [0004] In the prior art, Beilstan 16 898-899 has reported to react with the ether solution of p-bromophenethyl ether and bismuth-sodium alloy, extract with ether, and recrystallize with ethanol to prepare the method for tris (4-ethoxyphenyl) bismuth, yield was 51%. The preparation method uses bismuth-sodium alloy as the reaction raw material, and its preparation needs to react with metal bismuth and sodium, and ether is used as a solvent, which is highly toxic and prone to explosion, and the safety of the operation process is poor, the reaction time is long, the yield is low, and there is no industrial production. the value of. Contents of th...

Claims

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Application Information

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IPC IPC(8): C07F9/94
Inventor 袁振文廖本仁詹家荣
Owner SHANGHAI CHEM REAGENT RES INST
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