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Method for preparing indene-C60 bis-adduct by microwave reaction

A double adduct and microwave reaction technology, which is applied in chemical instruments and methods, hydrocarbons, hydrocarbons, etc., can solve the problem of cost reduction, long reaction cycle and low reaction selectivity of indene-C60 double adducts and other problems, to achieve the effect of increasing the chemical reaction rate, increasing the content, improving the reaction conversion rate and yield

Inactive Publication Date: 2012-05-30
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] However, the synthesis of indene-C in these prior art 60 There are fewer methods for double adducts, and there are some disadvantages. For example, Puplovskis et al. use o-dichlorobenzene as a solvent and need to react at a temperature greater than 180 ° C for 12 hours; Li Yongfang et al. use 1,2,4-trichlorobenzene As a solvent, it needs to be reacted at a temperature greater than 214 ° C for 12 hours, and indene-C 60 The highest yield of double adducts is only 34%
In these technologies, the reaction cycle is long and the reaction selectivity is too low, which is not conducive to the indene-C 60 The cost reduction of double adducts limits its large-scale production

Method used

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  • Method for preparing indene-C60 bis-adduct by microwave reaction
  • Method for preparing indene-C60 bis-adduct by microwave reaction

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Experimental program
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Effect test

Embodiment 1

[0019] Will C 60 Add 0.144 g (0.2 mmol), 0.463 g (4 mmol) of indene, and 10 ml of 1,2,4-trichlorobenzene into a three-necked flask equipped with a stirrer, condenser tube, and thermometer, stir well, and place in a microwave reaction In the reactor, under the protection of nitrogen, under the microwave radiation with a power of 800W, reacted for 30 minutes, the reaction system was settled by methanol, centrifuged, and the obtained brown solid was washed twice with methanol, and the VarianPro Star liquid chromatography was used. Analytical column (250×4.6 mm), with tetrahydrofuran and water (7:3) as the mobile phase, the analysis of indene-C 60 The conversion of the double adduct was 58.9%. Purified indene-C was obtained by silica gel column chromatography with toluene:n-hexane (1:200) as the eluent 60 Double adduct 78.06 mg, yield 41%.

Embodiment 2

[0021] Will C 60 Add 0.144 g (0.2 mmol), 0.463 g (4 mmol) of indene, and 10 ml of 1,2,4-trichlorobenzene into a three-necked flask equipped with a stirrer, condenser tube, and thermometer, stir well, and place in a microwave reaction In the reactor, under the protection of nitrogen, under the microwave radiation with a power of 800 W, the reaction system was reacted for 90 minutes. The reaction system was settled by methanol and centrifuged. Buckyprep analytical column (250×4.6 mm), using tetrahydrofuran and water (7:3) as mobile phase, analyzed to get indene-C 60 The conversion of the double adduct was 57.7%. Purified indene-C was obtained by silica gel column chromatography with toluene:n-hexane (1:200) as the eluent 60 Double adduct 76.54 mg, yield 40.2%.

Embodiment 3

[0023] Will C 60 Add 0.144 g (0.2 mmol), 0.463 g (4 mmol) of indene, and 10 ml of 1,2,4-trichlorobenzene into a three-necked flask equipped with a stirrer, condenser tube, and thermometer, stir well, and place in a microwave reaction In the reactor, under the protection of nitrogen, under the microwave radiation with a power of 1000 W, reacted for 30 minutes. The reaction system was settled by methanol and centrifuged. Buckyprep analytical column (250×4.6mm), with tetrahydrofuran and water (7:3) as the mobile phase, the conversion rate of indene-C60 double adduct was analyzed to be 56.3%. Purified indene-C was obtained by silica gel column chromatography with toluene:n-hexane (1:200) as the eluent 60 Double adduct 71.59 mg, yield 37.6%.

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Abstract

The invention discloses a method for preparing indene-C60 bis-adduct by microwave reaction, and is characterized by comprising the following steps: putting C60 and indene into a three-mouth bottle with a stirrer, a condenser pipe and a thermometer; adding solvent and evenly mixing; putting the mixture in a microwave reactor, wherein the molar ratio of C60 to indene is 1:5-1:50; under the protection of nitrogen, and reacting for 5 minutes-2 hours while stirring under the radiation of microwave of which the power is 300-1000 W; and purifying after methanol settlement to obtain the indene-C60 bis-adduct. The method has low energy consumption, quick reaction and higher reaction percent conversion and yield and can shorten reaction time.

Description

technical field [0001] The invention belongs to the preparation in the field of organic chemical industry, specifically a method for preparing indene-C by using microwave reaction 60 Double adduct method. Background technique [0002] Since 1995, Yu Gang discovered that polyphenylene vinylene derivatives and fullerenes (C 60 ) since the ultrafast charge transport between the C 60 It and its derivatives have been identified as ideal electron acceptor materials in polymer bulk heterojunction thin film photovoltaic cells due to their high electron mobility and electron affinity. but C 60 Poor solubility in organic solvents restricts the preparation of bulk heterojunction thin films. To improve C 60 Solubility in organic solvents, C obtained by introducing substituents on its surface 60 Derivatives such as [6,6]-phenyl-C 61 - Methyl butyrate (PC 61 BM) and [6,6]-phenyl-C 71 - Methyl butyrate (PC 71 BM), which has good solubility in chloroform, tetrahydrofuran, toluene,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C13/64C07C2/00
Inventor 高潮陈冬刘建群丛志远贾林杜渭松刘红利蒋忠亮
Owner XIAN MODERN CHEM RES INST