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Preparation method of hexa(4-methoxyphenoxyl)cyclotriphosphazene

A technology of methoxyphenoxy and hexachlorocyclotriphosphazene, which is applied in the field of preparation of hexacyclotriphosphazene, can solve the problems of complex post-processing and long reaction time, and achieve easy control of reaction conditions and high yield , the effect of mild reaction conditions

Inactive Publication Date: 2015-01-28
NO 53 RES INST OF CHINA NORTH IND GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method has a long reaction time and complex post-processing

Method used

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  • Preparation method of hexa(4-methoxyphenoxyl)cyclotriphosphazene
  • Preparation method of hexa(4-methoxyphenoxyl)cyclotriphosphazene
  • Preparation method of hexa(4-methoxyphenoxyl)cyclotriphosphazene

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Experimental program
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Effect test

Embodiment 1

[0028] Add 12ml of acetone and 1.2g (30mmol) of sodium hydride (60%) into a 250ml round-bottomed flask, slowly add 15ml of acetone solution with 3.72g (30mmol) of p-hydroxyanisole dropwise, 800W ultrasonic for 10min, and place Add dropwise 22ml of acetone solution containing 1.74g (5mmol) hexachlorocyclotriphosphazene into a round-bottomed flask under ultrasonication. After the dropwise addition, ultrasonicate at 800W and 45°C for 1h, reflux for 11.5h, and distill under reduced pressure after the reaction is completed. Remove the solvent in the system to obtain a light yellow turbid viscous liquid, then add 30ml of dichloromethane dropwise to the viscous liquid, wash with deionized water until the water phase is neutral, separate the liquids and dry the organic phase with anhydrous magnesium sulfate for 5min, reduce Dichloromethane was evaporated under pressure to obtain hexa(4-methoxyphenoxy)cyclotriphosphazene with a yield of 89.3%.

[0029] The molecular formula of hexa(4-m...

Embodiment 2

[0031] 17ml of tetrahydrofuran and 1.41g (35.25mmol) of sodium hydride (60%) were added to a 250ml round-bottomed flask, and 15ml of tetrahydrofuran solution containing 4.37g (35.25mmol) of p-hydroxyanisole was slowly added dropwise, followed by ultrasonication at 950W for 15min, and then Add dropwise 14ml of tetrahydrofuran solution containing 1.74g (5mmol) hexachlorocyclotriphosphazene to a round-bottomed flask placed in ultrasonication. After the addition is completed, ultrasonicate at 950W and 55°C for 2h, reflux for 12h, and depressurize after the reaction is completed. Distill the liquid after the reaction to obtain a light yellow turbid viscous liquid, then add 30ml of dichloromethane dropwise to the viscous liquid, wash the above liquid with deionized water to neutrality, separate the liquids to get the organic phase, dry it with anhydrous magnesium sulfate for 5min, reduce The solvent dichloromethane was evaporated under pressure to obtain hexa(4-methoxyphenoxy)cyclotr...

Embodiment 3

[0034] Add 20ml of acetone and 1.92g (48mmol) of sodium hydride (60%) into a 250ml round-bottomed flask, slowly add 20ml of tetrahydrofuran solution containing 4.96g (40mmol) of p-hydroxyanisole dropwise, 900W ultrasonic for 20min, and place Add dropwise 12ml of dioxane solution containing 1.74g (5mmol) hexachlorocyclotriphosphazene to a round-bottomed flask under ultrasonication. After the addition is completed, ultrasonicate at 850W and 40°C for 2.5h, and reflux for 11h. After the reaction is completed, Distill the reaction liquid under reduced pressure to obtain a light yellow turbid viscous liquid, then add 30ml of dichloromethane dropwise to the viscous liquid, wash the above liquid with deionized water until neutral, separate the liquids to take the organic phase, and dry it with anhydrous calcium chloride After 30 minutes, dichloromethane was evaporated under reduced pressure to obtain hexa(4-methoxyphenoxy)cyclotriphosphazene with a yield of 93.1%.

[0035] 1 H-NMR (D...

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Abstract

The invention belongs to the technical field of organic synthesis. An ultrasonic vibration technology is adopted to accelerate the movement of chemical balance to a product direction. The invention relates to a preparation method of hexa(4-methoxyphenoxyl)cyclotriphosphazene. The method comprises a salt forming process, a nucleophilic substitution process and a post-treatment process, and concretely comprises the following steps: adding a 4-methoxyphenol solution into an acid binding agent solution in a dropwise manner under 800-1000W ultrasonic conditions, and reacting at room temperature for 10-30min to obtain a 4-methoxyphenol salt solution; adding a hexachlorocyclotriphosphazene solution into the 4-methoxyphenol salt solution in a dropwise manner under 800-1000W ultrasonic conditions, and reacting at 35-60DEG C for 1-4h; carrying out a refluxing reaction for 8-12h to obtain a hexa(4-methoxyphenoxyl)cyclotriphosphazene solution; and carrying out reduced pressure distillation to evaporate a solvent in the obtained system, dissolving the obtained concentrated in dichloromethane, washing by deionized water, drying, and carrying out reduced pressure distillation to obtain the target product hexa(4-methoxyphenoxyl)cyclotriphosphazene. The preparation method has the advantages of mildness and easy control of reaction conditions, and high yield, and is suitable for preparing hexa(4-methoxyphenoxyl)cyclotriphosphazene.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis and relates to the preparation technology of hexa(4-methoxyphenoxy)cyclotriphosphazene. Background technique [0002] Hexa(4-methoxyphenoxy)cyclotriphosphazene is a cyclotriphosphazene derivative containing a benzene ring, which can be used as a modifier for heat-resistant and flame-retardant resins; in addition, hexa(4-methoxy Phenyloxy)cyclotriphosphazene is an important intermediate for the preparation of star compounds. [0003] US00552319A has synthesized six (4-methoxyphenoxy) cyclotriphosphazene as raw material with hexachlorocyclotriphosphazene, p-hydroxyanisole and acid-binding agent (sodium hydride, triethylamine), and its technique is to Hexachlorocyclotriphosphazene, acid-binding agent and tetrahydrofuran are placed in a flask, and the tetrahydrofuran solution of p-hydroxyanisole is added dropwise to the flask, and then the temperature is raised to reflux for 24 hours; after...

Claims

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Application Information

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IPC IPC(8): C07F9/6593
Inventor 高岩立冀克俭刘元俊张彬赵晓刚周彤李艳玲邵鸿飞邓卫华华兰
Owner NO 53 RES INST OF CHINA NORTH IND GRP
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