Preparation method of acetyl cyclopentadienyl iron

A kind of acetyl ferrocene, said technology, applied in the direction of chemical instruments and methods, metallocene, organic chemistry, etc., can solve the problems of unsatisfactory industrialization prospects, difficult post-processing separation, cumbersome operation, etc., and achieve the elimination of purification operation Steps, inhibition of side reactions, good product purity

Inactive Publication Date: 2007-04-18
SHANGHAI CHEM REAGENT RES INST
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The object of the present invention is to provide a kind of preparation method of acetyl ferrocene, to overcome the diacetylated by-product of acetylation reaction in the prior art, difficult post-treatment separation, high cost, cumbersome operation, much waste water, and poor industrialization prospect Ideal Disadvantages

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  • Preparation method of acetyl cyclopentadienyl iron
  • Preparation method of acetyl cyclopentadienyl iron

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Experimental program
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Effect test

Embodiment 1

[0020] Add 125ml of dichloromethane reaction solvent in the 500ml four-port reactor with cooling, thermometer, stirrer, gas inlet tube, add 0.1mol (18.6g) ferrocene under stirring, import nitrogen, under nitrogen atmosphere, cool to -8°C, within 3 hours, slowly drop into the mixed solution composed of the acetylation reagent acetyl chloride and the binary catalyst solution. g) Anhydrous aluminum trichloride, 0.0107mol (1.52g) 47% boron trifluoride ether solution>, warm up to 20°C, maintain the temperature for 3 hours, add 10ml of water dropwise under stirring, filter, evaporate the reaction solvent, 20ml of 30-60°C petroleum ether was added, yellow crystals were precipitated, and dried to obtain 21.1 g of acetylferrocene, with a yield of 92.0%, a purity of 99.3% (HPLC), and a melting point of 86-87°C.

Embodiment 2

[0022] Add 125ml of dichloromethane into a 500ml four-port reactor with cooling, thermometer, stirrer, and gas inlet tube, add 0.1mol (18.6g) of ferrocene under stirring, introduce nitrogen, and cool to 0°C under nitrogen atmosphere , within 4 hours, drop the mixed solution of the acetylation reagent acetyl chloride and the binary catalyst solution. Aluminum trichloride, 0.02mol (2.84g) 47% boron trifluoride ether solution>, warming up to 20°C, maintaining the temperature for 2 hours, adding 10ml of water dropwise under stirring, filtering, distilling off the reaction solvent, adding 20ml of 30 Petroleum ether at -60°C precipitated yellow crystals and dried to obtain 20.4 g of acetylferrocene, with a yield of 89.1%, a purity of 98.3% (HPLC), and a melting point of 85-87°C.

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Abstract

The present invention discloses a method for preparing acetylferrocene. Said method includes the following steps: using ferrocene as raw material, making said ferrocene and solution formed from acetylation reagent and binary catalyst produce reaction in haloolefin reaction solvent so as to obtain the invented target product whose purity can be up to above 98% and yield is 89-92%.

Description

technical field [0001] The invention relates to a preparation method of acetyl ferrocene. Background technique [0002] Acetyl ferrocene is a raw material for preparing ferrocene derivatives, especially as an intermediate for preparing solid fuel burning rate catalysts. Its structural formula is: [0003] [0004] In the prior art, Li Baoguo et al. have disclosed a method for preparing acetyl ferrocene using ferrocene as a raw material, dichloromethane as a reaction solvent, anhydrous aluminum chloride as a catalyst, and acetyl chloride as an acetylation reagent. (Chemical Reagents, 2001, 23 (5): 292-293), the yield of this method is 81.5%, there is diacetylated compound by-product to generate in the reaction process, and the reaction product needs to use the method for column to separate, does not have application value. [0005] R.D.Vukicevic etc. used ferrocene as raw material, dichloromethane as reaction solvent, anhydrous aluminum trichloride as catalyst, acetic ac...

Claims

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Application Information

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IPC IPC(8): C07F17/02
Inventor 施沁清吕蔚蒋旭亮
Owner SHANGHAI CHEM REAGENT RES INST
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