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Method of synthesizing alkylated ferrocene derivative

A technology for alkylating ferrocene and ferrocene derivatives, applied in chemical instruments and methods, metallocenes, organic chemistry, etc., can solve problems such as large environmental impact and complicated process steps, and achieve high selectivity

Active Publication Date: 2017-08-04
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing process steps for the synthesis of alkylated ferrocene derivatives using ferrocene are complicated and have a great impact on the environment

Method used

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  • Method of synthesizing alkylated ferrocene derivative

Examples

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Effect test

Embodiment 1

[0038] In this example, ferrocene is used as raw material, phosphoric acid supported on silica gel (loading capacity 25%) is used as catalyst, toluene is used as solvent, and isobutanol is used as alkylating agent.

[0039] Reactor volume: 100ml

[0040] Ferrocene: 2g

[0041] Catalyst: 1g

[0042] Alkylating agent: 4g

[0043] Toluene: 20ml

[0044] Reaction temperature: 120°C

[0045] Nitrogen pressure: 1MPa

[0046] Response time: 4h

[0047] Stirring rate: 500r / min

[0048] The reaction was carried out in a 100ml autoclave. Before the reaction, nitrogen gas was filled and discharged several times to replace the residual air in the still body, and 1MPa nitrogen gas was charged to maintain the high-pressure environment in the still. Stir and raise to the reaction temperature of 120°C at a rate of 5°C / min. After reacting for 4 hours, stop heating, slowly release nitrogen after cooling, and filter to obtain the filtrate as the mixture of raw materials and products. Th...

Embodiment 2

[0051] In this example, ferrocene is used as raw material, phosphoric acid supported on silica gel (loading capacity 50%) is used as catalyst, trimethylbenzene is used as solvent, and isobutylene is used as alkylating agent.

[0052] Reactor volume: 100ml

[0053] Ferrocene: 2g

[0054] Catalyst: 1g

[0055] Alkylating agent: 8g

[0056] Trimethylbenzene: 20ml

[0057] Reaction temperature: 180°C

[0058] Nitrogen pressure: 1MPa

[0059] Response time: 4h

[0060] Stirring rate: 500r / min

[0061] The reaction was carried out in a 100ml autoclave. Before the reaction, nitrogen gas was filled and discharged several times to replace the residual air in the still body, and 1MPa nitrogen gas was charged to maintain the high-pressure environment in the still. Stir and raise to a reaction temperature of 180°C at a rate of 5°C / min. After reacting for 4 hours, stop heating, slowly release nitrogen after cooling, and filter to obtain the filtrate as the mixture of raw materials ...

Embodiment 3

[0064] In this example, ferrocene is used as raw material, phosphoric acid supported on silica gel (loading capacity 75%) is used as catalyst, toluene is used as solvent, and tert-butanol is used as alkylating agent.

[0065] Reactor volume: 100ml

[0066] Ferrocene: 2g

[0067] Catalyst: 1g

[0068] Alkylating agent: 2g

[0069] Toluene: 20ml

[0070] Reaction temperature: 230°C

[0071] Nitrogen pressure: 1MPa

[0072] Response time: 4h

[0073] Stirring rate: 500r / min

[0074] The reaction was carried out in a 100ml autoclave. Before the reaction, nitrogen gas was filled and discharged several times to replace the residual air in the still body, and 1MPa nitrogen gas was charged to maintain the high-pressure environment in the still. Stir and raise to reaction temperature 230°C at a rate of 5°C / min. After reacting for 4 hours, stop heating, slowly release nitrogen after cooling, and filter to obtain the filtrate as the mixture of raw materials and products. The mix...

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Abstract

The invention discloses a method of synthesizing an alkylated ferrocene derivative; the method comprises: mixing ferrocene, an alkylation reagent, an organic solvent and a supported solid catalyst, adding the mixture into a high-pressure reactor, charging nitrogen at normal temperature to 0.5-2.5 MPa, sealing, heating to 80-250 DEG C, and stirring for reacting for 2-6 h; after reacting, filtering the reaction mixed liquid, vacuum-distilling the filtrate, and concentrating to obtain the alkylated ferrocene derivative. The defects that traditional process products are difficult to separate and reuse and cause high pollution and corrosion are overcome. The obtained alkylated ferrocene derivative is applicable to diesel combustion supporting, emission particulate matter trap regeneration and other fields.

Description

[0001] This application is the application number 2014105213428, the application date is September 30, 2014, and the name is a divisional application of the patent application for the synthesis method of alkylated ferrocene derivatives technical field [0002] The invention relates to a method for synthesizing alkylated ferrocene derivatives by using a solid acid catalyst. Background technique [0003] Ferrocene, also known as dicyclopentadienyl iron, is a metal-organic compound with a sandwich structure. It is orange crystalline at room temperature, insoluble in water, and easily soluble in organic solvents such as diesel, gasoline, benzene, and ethanol. It has the characteristics of stable chemical properties, odorless and non-toxic. Because ferrocene and its derivatives are widely used, they are often used in liquid fuels such as gasoline, diesel oil, and heavy diesel oil as smoke-elimination and energy-saving additives, which have obvious effects on energy saving, smoke ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F17/02
CPCC07F17/02
Inventor 张泽凯王成曾高翔刘华彦卢晗锋陈银飞
Owner ZHEJIANG UNIV OF TECH
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