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Synthetic technology of novel material intermediate alkyl viologen diperchlorate

A perchlorate and new material technology, applied in the field of materials, can solve the problems such as the synthesis process of alkyl viologen diperchlorate that has not been reported, and achieve the effect of low cost and simple operation

Inactive Publication Date: 2013-04-10
SUZHOU BAILINGWEI HYPERFINE MATERIAL
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] But the specific synthesis technique of alkyl viologens diperchlorate is not all reported in the known literature now

Method used

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  • Synthetic technology of novel material intermediate alkyl viologen diperchlorate
  • Synthetic technology of novel material intermediate alkyl viologen diperchlorate

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Embodiment 1

[0025] The first step reaction: preparation of intermediate ethyl viologen dibromide

[0026] Add 4,4'-bipyridine (31.2g, 200mmol, 1eq), bromoethane (150mL, 2mol, 10eq) and acetonitrile (300mL) into a 1L three-necked reaction flask, and heat the reaction solution to reflux (about 80°C), After the reaction was completed, the heating was stopped. The reactant was cooled to 10°C with an additional ice-water bath, stirred for 1 hour, and filtered with suction. The filter cake was washed successively with dichloromethane (200mL), acetone (100mL) and n-hexane (200mL), drained, and vacuum-dried to obtain 66.7g yellow crystal ethyl viologen dibromide, yield: 90%, purity : 99.4%. Melting point: 278°C

[0027] The second step reaction: preparation of ethyl viologen diperchlorate

[0028] Aqueous perchloric acid solution (150mL, 70%, 7.78eq) and ethyl viologen dibromide (50.0g, 134.4mmol, 1eq) were added to a 2L four-necked reaction flask, and the reaction solution was heated to refl...

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Abstract

The invention relates to a synthetic technology of a novel material intermediate alkyl viologen diperchlorate importantly used for electrochromic and conductive compounds / devices. The synthetic technology comprises the following steps: heating 4,4'-dipyridine and alkylogen in an acetonitrile solution for refluxing until reaction completing, cooling for crystallization, carrying out pumping filtration, respectively and sequentially washing the obtained filter cake by dichloromethane, acetone and n-hexane, draining, and carrying out vacuum drying to obtain alkyl viologen dihalide; and heating the alkyl viologen dihalide and an aqueous solution of perchloric acid to reflux, cooling for crystallization after reaction completing, washing the obtained crude alkyl viologen diperchlorate by acetone, draining, and carrying out vacuum drying to obtain the alkyl viologen diperchlorate. The technology has the advantages of easily available initial raw materials, short reaction step, operation convenience, high yield and low cost.

Description

technical field [0001] The invention belongs to the field of materials, in particular to a synthesis process of an intermediate alkyl viologen diperchlorate used in electrochromic materials and conductive composites / device materials. Background technique: [0002] Alkyl viologen diperchlorate is an important class of material intermediates for electrochromic and conductive composites / devices, such as Wu, Jin reported the synthesis of polyaniline composites based on ethyl viologen diperchlorate Conductive applications (US20100190956), PozoGonzalo, Cristina et al. reported that the compound based on alkyl viologen diperchlorate realized electrochromism at room temperature, which can be used for electrochromic materials such as all-plastic, all-transparent thermosensitive substrates. Chromogenic devices (US20110003070). Therefore, alkyl viologen diperchlorate has a good market prospect as a material intermediate with electrochromic and conductive composites / devices. [0003] ...

Claims

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Application Information

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IPC IPC(8): C07D213/22C07D213/127
Inventor 宋绍兴邹增龙顾扬王喆
Owner SUZHOU BAILINGWEI HYPERFINE MATERIAL
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