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Production method of ethylferrocene

A technology of ethyl ferrocene and production method, which is applied in chemical instruments and methods, metallocene, organic chemistry, etc., to achieve the effects of avoiding incomplete reaction, simple treatment, and eliminating pollution

Inactive Publication Date: 2015-09-30
JIAXING ZHENGDA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] For the above-mentioned problems existing in the prior art, the object of the present invention is to provide a kind of method that pollutes less, yield is high, simple to operate and prepare ethyl ferrocene with ferrocene through acylation, reduction reaction, and this method can Solve problems such as yield and environmental pollution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Ferrocene 98.5% (content) 750g, dispersant dichloroethane 3000g, put into the stirred reactor; dropwise add 85% concentrated phosphoric acid 503g, acetic anhydride 491g, maintain the reaction temperature at 50°C, neutralize and rinse with 200g sodium bicarbonate After 3 times, separate the dispersant; put the dispersant layer into the stirring reactor, add 1500g of zinc tin alkaloid (the mass ratio of zinc powder to stannous chloride is 10:1), 1L of isopropanol, and 5.5L of hydrochloric acid to maintain the reaction The temperature is 60-80°C. During the reaction, use liquid chromatography to track and retrieve the content of acyl ferrocene. When the content is lower than 0.5%, filter and rinse after the reaction; distill the dispersant at a temperature of 70-75°C. After the end, use 200g of sodium sulfate was dried to obtain 790g of product, with a yield of 91.7%, and the content measured by liquid chromatography was 99.2%.

Embodiment 2

[0027] Ferrocene 98.5% (content) 750g, dispersant toluene 2250g, put into the stirred reactor; dropwise add 85% concentrated phosphoric acid 503g, acetic anhydride 491g, maintain the reaction temperature at 50°C, neutralize and rinse with 200g sodium bicarbonate for 3 times Separate the dispersant; put the dispersant layer into the stirred reactor, add 1500g of zinc tin alkaloid (the mass ratio of zinc powder to stannous chloride is 10:1), 1L of isopropanol, 5.5L of hydrochloric acid, and maintain the reaction temperature at 60- 80°C, filter and rinse after the reaction; distill the dispersant at a temperature of 70-75°C, and dry with 200g of sodium sulfate to obtain 774g of the product, with a yield of 89.8% and a content of 99.01%.

Embodiment 3

[0029] Ferrocene 98.5% (content) 750g, dispersant toluene 3000g, put into the stirring reactor; dropwise add 85% concentrated phosphoric acid 491g, acetic anhydride 503g, maintain the reaction temperature at 50°C, neutralize and rinse with 200g sodium bicarbonate for 3 times Separate the dispersant; put the dispersant layer into the stirred reactor, add 1500g of zinc tin alkaloid (the mass ratio of zinc powder to stannous chloride is 11:1), 1L of isopropanol, 5.5L of hydrochloric acid, and maintain the reaction temperature at 60- 80°C, filter and rinse after the reaction; distill the dispersant at a temperature of 70-75°C, and dry with 200g of sodium sulfate to obtain 754g of the product, with a yield of 87.5% and a content of 89.99%.

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Abstract

Belonging to the technical field of ethylferrocene synthesis, the invention relates to a production method of ethylferrocene. The method includes: taking ferrocene as the raw material, in the presence of a dispersing agent and a catalyst, subjecting the raw material and an acylating agent to acylation reaction to obtain acetylferrocene, and carrying out reduction reaction on the acetylferrocene and a reduction agent zinc tin alloy to obtain ethylferrocene. The method provided by the invention adopts an inert organic solvent as the dispersing agent and takes non-toxic zinc tin alloy as the reducing agent, so that the incomplete reaction problem caused by nonuniform reaction system can be avoided, at the same time the neutralization, filtration and drying steps are omitted, and pollution brought about by existing reduction agent zinc tin alloy waste liquid is completely eradicated, the treatment becomes simpler, and the yield is enhanced. According to the method, the yield of ethylferrocene is up to over 87.5%, and the content reaches over 99%.

Description

technical field [0001] The invention belongs to the technical field of ethyl ferrocene synthesis, and in particular relates to a production method of ethyl ferrocene obtained by sequentially acylation and alkylation reactions using ferrocene as a raw material. Background technique [0002] The molecule of ethylferrocene is polar, and has high thermal stability, chemical stability and radiation resistance, and it also has a wide range of applications in industry, agriculture, medicine, aerospace, energy saving, environmental protection and other industries. However, due to the yield of the synthesis process and the problems of the three wastes, the production cost is high and the three wastes are serious, the industrialization has not been truly realized, and the application is limited. The usual preparation method of ethyl ferrocene is to acylate ferrocene with acetic anhydride under the catalysis of phosphoric acid, and the yield is about 82%; under the catalysis of boron t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F17/02
CPCC07F17/02
Inventor 杨丽艳季金华张鹏飞史迎军陶明泉
Owner JIAXING ZHENGDA CHEM
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