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Monoacyl ferrocene Schiff base aminocyclotriphosphazene and its synthesis method

A kind of technology of monoacyl ferrocene Schiff base amino cyclotriphosphazene and monoacyl ferrocene Schiff base amino group, which is applied in the field of monoacyl ferrocene Schiff base amino cyclotriphosphazene and its synthesis , can solve the problems of difficult preparation, low reaction temperature, inconvenient operation, etc., and achieve the effect of low cost

Inactive Publication Date: 2011-12-14
SHANGHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The literature (J.Am.Chem.Soc.1984, 106, 2337~2347) reports that ferrocene reacts with organic lithium to prepare ferrocene lithium at low temperature, and ferrocene lithium reacts with hexachlorocyclotriphosphazene or Hexafluorocyclotriphosphazene nucleophilic substitution reaction to synthesize ferrocene cyclotriphosphazene derivatives. The raw materials used in the route are not easy to obtain; the reaction temperature is low and the operation is inconvenient

Method used

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  • Monoacyl ferrocene Schiff base aminocyclotriphosphazene and its synthesis method
  • Monoacyl ferrocene Schiff base aminocyclotriphosphazene and its synthesis method

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Embodiment 1

[0030] Embodiment 1: The synthesis of monoacyl ferrocene Schiff base aminocyclotriphosphazene is realized through the following steps:

[0031] Synthesis of hexachlorocyclotriphosphazene: In a 500ml four-necked flask equipped with a mechanical stirrer, a condenser, and a thermometer, add finely ground ammonium chloride 30g, 120ml chlorobenzene, 1g zinc oxide, and 20ml pyridine in sequence, and heat and stir To the reflux of chlorobenzene. Then slowly drop into the chlorobenzene solution dissolved with 100g of phosphorus pentachloride for about 2 hours, keep the solution under reflux for 2 to 3 hours until the HCl in the airway tube is obviously weakened and stop heating. Continue stirring to discharge the HCl gas in the system, cool the reaction system, and filter to obtain a light yellow solution. Wash the solution with distilled water for 2 to 3 times until the organic layer is clear and transparent, separate the chlorobenzene layer, add anhydrous sodium sulfate to dry ov...

Embodiment 2

[0037] The synthesis of monoacyl ferrocene Schiff base amino cyclotriphosphazene is realized through the following steps:

[0038] Synthesis of hexachlorocyclotriphosphazene: In a 500ml four-necked flask equipped with a mechanical stirrer, a condenser, and a thermometer, add finely ground 30g ammonium chloride, 120ml chlorobenzene, 1g anhydrous magnesium chloride, and 20ml pyridine in turn, and heat Stir until the chlorobenzene refluxes. Then slowly drop into the chlorobenzene solution dissolved with 100g of phosphorus pentachloride for about 2 hours, keep the solution under reflux for 2 to 3 hours until the HCl in the airway tube is obviously weakened and stop heating. Continue stirring to discharge the HCl gas in the system, cool the reaction system, and filter to obtain a light yellow solution. Wash the solution with distilled water for 2 to 3 times until the organic layer is clear and transparent, separate the chlorobenzene layer, add anhydrous sodium sulfate to dry ove...

Embodiment 3

[0044] The synthesis of monoacyl ferrocene Schiff base amino cyclotriphosphazene is realized through the following steps:

[0045] Synthesis of hexachlorocyclotriphosphazene: In a 500ml four-neck flask equipped with a mechanical stirrer, a condenser, and a thermometer, add finely ground 30g ammonium chloride, 200ml tetrachloroethane, 1g anhydrous zinc chloride, 20ml of pyridine, heated and stirred until tetrachloroethane refluxed. Then add 100g of phosphorus pentachloride in 5 to 10 times, and finish adding in about 2 hours, keep the solution under reflux for 2 to 3 hours, and stop heating when the HCl in the airway tube is obviously weakened. Continue stirring to discharge the HCl gas in the system, cool the reaction system, and filter to obtain a light green solution. Wash the solution with distilled water for 2 to 3 times until the organic layer is clear and transparent, separate the tetrachloroethane layer, add anhydrous sodium sulfate to dry overnight, filter, and dist...

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Abstract

The invention relates to a monoacyl ferrocene Schiff base aminocyclotriphosphazene and a synthesis method thereof. The structural formula of the compound is: the present invention makes the prepared monoacyl ferrocene Schiff base amino cyclotriphosphazene have the advantages of ferrocene group and cyclotriphosphazene matrix at the same time, and shows special performance. It has a wide range of application values ​​in chemistry, medicine, catalyst, lubrication and other fields. Compared with the prior art, the method for introducing the ferrocene group into the cyclotriphosphazene matrix of the present invention avoids highly active reagents such as butyllithium, can be operated at normal temperature, and has a simple, safe and low-cost method. features.

Description

technical field [0001] The invention relates to a monoacyl ferrocene Schiff base aminocyclotriphosphazene and a synthesis method thereof. Background technique [0002] The ferrocene group has aromaticity, redox property and low toxicity, and its Schiff base has a wide range of applications in polymers, electrochemistry, medicine, catalysts and other fields. Introducing ferrocene groups into different molecules in order to obtain new compounds or compounds with special properties is a hot spot in the research of ferrocene chemistry in recent years. Polyphosphazene is a general term for a series of polymers whose main chain consists of nitrogen and phosphorus atoms alternating single and double bonds, and organic substituents are side chains. By choosing different side chain substituents, various phosphazene Schiff bases with different properties can be prepared. Its properties are between inorganic compounds, organic compounds and polymers, and it is called "inorganic rubber...

Claims

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Application Information

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IPC IPC(8): C07F19/00C07F17/02C07F9/6593
Inventor 郭强聂智军赵正平孙金亮张四刚刘海彬潘国梁
Owner SHANGHAI UNIV
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