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Synthetic method of intermediate diacetyl ferrocene

A technology of bisacetylferrocene and synthesis method, applied in chemical instruments and methods, metallocenes, catalysts for physical/chemical processes, etc., can solve the problems of difficult control of reaction conditions, unsatisfactory yield, mild reaction conditions and the like

Active Publication Date: 2020-07-07
徐州邦博信息科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because strong acetylating reagents such as acetic anhydride and Lewis acid anhydrous aluminum trichloride are used as catalysts, this reaction is easier to carry out, but the side reactions are complicated and produce a variety of by-products that are difficult to separate. The equipment requirements are very high, the reaction conditions are difficult to control in the production process, and the reaction conditions are mild, the reaction time is too long, and the yield is not ideal. In order to overcome the above disadvantages, it is necessary to provide a new synthesis process for Improving the efficiency of the production of bisacetylferrocene intermediates

Method used

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  • Synthetic method of intermediate diacetyl ferrocene

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Embodiment 1

[0019] 1, a kind of synthetic method of intermediate bisacetyl ferrocene, it is characterized in that the method comprises the following steps:

[0020] Step 1. Dissolve 4g of ferrocene and 5g of acetic anhydride in 80ml of toluene in a four-necked flask. After fully dissolving, transfer it to a supercritical device, and feed supercritical carbon dioxide fluid into it, slowly at a rate of 0.5°C / min Heat up, add 8g AlCl 3 The loaded A1-MCM-41 catalyst was stirred at a constant temperature of 40°C and 7.5MPa for 5min;

[0021] Step 2. Add 30ml of chloroform under ultrasonic vibration conditions to make the catalyst fully dispersed and dissolved, and the reactor is connected to a tail gas absorption device that can prevent sucking back;

[0022] Step 3. Continue to feed supercritical carbon dioxide fluid into the reaction device, keep it at 0°C and 7.5Mpa, and the solution will turn blood red after 15 minutes, and the acetylation reaction will be completed when the solution turn...

Embodiment 2

[0033] Step 1. Dissolve 3g of ferrocene and 5g of acetic anhydride in 80ml of toluene in a four-neck flask. After fully dissolving, transfer it to a supercritical device, and feed supercritical carbon dioxide fluid into it, slowly at a rate of 0.5°C / min Heat up, add 8g AlCl 3 The supported A1-MCM-41 catalyst was stirred at a constant temperature of 40° C. and 7.5 MPa for 5 minutes; the rest of the steps were the same as in Example 1.

Embodiment 3

[0035] Step 1. Dissolve 2g of ferrocene and 5g of acetic anhydride in 80ml of toluene in a four-neck flask. After fully dissolving, transfer it to a supercritical device and feed supercritical carbon dioxide fluid. Slowly Heat up, add 8g AlCl 3 The supported A1-MCM-41 catalyst was stirred at a constant temperature of 40° C. and 7.5 MPa for 5 minutes; the rest of the steps were the same as in Example 1.

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Abstract

The invention discloses a synthesis method of an intermediate diacetyl ferrocene, which comprises the following steps: taking ferrocene, acetic anhydride, trichloromethane, AlCl3, aluminum isopropoxide, tetraethylammonium hydroxide and tetraethoxysilane as main raw materials, wherein proportions of the following raw materials are: ferrocene and acetic anhydride in a mass ratio of 4: 5; the molar ratio of SiO2 to Al2O3 is 60: 1; the mass ratio of Al-MCM-41 to AlCl3 is 7: 2; according to the synthesis process, a low-temperature supercritical fluid process is adopted to catalyze an acylation reaction of ferrocene and acetic anhydride to prepare high-purity diacetyl ferrocene. And under the shape-selective catalysis of A1-MCM-41, the selectivity and the yield of the product can be greatly improved, so that the production efficiency of the intermediate is improved.

Description

technical field [0001] The invention relates to a method for synthesizing an intermediate bisacetyl ferrocene, which belongs to the field of chemical synthesis. Background technique [0002] Diacetylferrocene (Diacetylferrocene) CAS: 1273-94-5, etc., is an important raw material and intermediate for the synthesis of ferrocene derivatives, and has a wide range of applications in functional materials, polymers, electrochemistry, medicine, catalysis, etc. application. The synthesis of ferrocene diacetylation is through two synthetic approaches: under the catalysis of anhydrous aluminum trichloride, the one is solvent with ethylene dichloride, the acylating agent with corresponding acyl chloride, the other is with chloroform As a solvent, acid anhydride is used as an acylating agent. Since a strong acetylating reagent such as acetic anhydride and Lewis acid anhydrous aluminum trichloride are used as catalysts, the reaction is easier to carry out, but the side reactions are com...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F17/02B01J29/04
CPCC07F17/02B01J29/041Y02P20/54Y02P20/141
Inventor 刘可王凡
Owner 徐州邦博信息科技有限公司
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