A kind of preparation technology of cobalt dicene

A preparation process and technology of cobaltene, which is applied in the field of preparation technology of metal compound cobaltene, can solve problems such as unmentioned product purity, and achieve the effects of low production cost, wide source, simple and safe operation

Active Publication Date: 2019-03-12
ZUNYI MEDICAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition, in the above-mentioned prior art, what patent CN101108366A obtains is a mixture of cobaltocene, acetonitrile and the generated impurities; and the post-treatment means of patent CN101108366A after the reaction is completed is only a simple operation of filtration and distillation, and does not mention product purity

Method used

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  • A kind of preparation technology of cobalt dicene
  • A kind of preparation technology of cobalt dicene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] 1) Add 97.79ml of methanol dropwise to 41.58g of sodium methoxide, and use nitrogen gas bubbling for 5 minutes to remove the oxygen in the solvent. During the dropwise addition, the solution is cooled and the temperature is maintained at 40°C. Then add a mixed solution of 20 g of anhydrous cobalt dichloride and 63.91 ml of methanol, feed for about 15 minutes, continue to stir for 30 minutes, and react for 5 hours to obtain a methanol solution mixture of anhydrous cobalt methoxide;

[0031] 2) Add 32.95ml of cyclopentadiene monomer and 33.11ml of methanol solution dropwise at 40-45°C, feed for about 30 minutes, and then stir for about 5 hours to obtain a methanol mixture of cobaltocene;

[0032] 3) Rotate the mixed solution to remove the solvent to obtain the crude cobalt dicene, add 100ml of toluene to the crude product, after repeated shaking, filter and recover the filtrate, then spin off the filtrate, add 150ml of petroleum ether, reflux for a while, spin off half of ...

Embodiment 2

[0034] 1) 10ml of ethanol was added dropwise into 5.24g of sodium ethoxide, and the oxygen in the solvent was removed by bubbling nitrogen gas for 5 minutes. During the dropwise addition, the solution was cooled and the temperature was maintained at 40°C. Then add a mixed solution of 2 g of anhydrous cobalt dichloride and 8 ml of ethanol, continue the feeding for about 15 minutes, continue stirring for 30 minutes, and react for 5 hours to obtain an ethanolic solution mixture of cobalt in anhydrous alcohol.

[0035] 2) Add 3.3ml of cyclopentadiene and 4ml of ethanol solution dropwise at 45-50°C for 30 minutes, and then stir for 5 hours to obtain a mixture of cobaltocene and ethanol;

[0036] 3) Rotate the mixed solution to remove the solvent, add 10ml of toluene to the residue, and after repeated shaking, filter and recover the filtrate, then spin off the filtrate, add 8ml of petroleum ether, reflux for a while, then cool, and crystallize in an ice-water bath , and filtered the...

Embodiment 3

[0038] The difference from Example 1 is that the reaction temperature in Step 1 is 30°C.

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Abstract

The invention provides a preparation technology of cobaltocene. The preparation technology comprises the following steps: (1) reacting cobalt dichloride with a metal compound containing alkyloxy in an oxygen-free first alcoholic solvent to obtain a cobalt compound containing alkyloxy; (2) reacting the alkyloxy-containing cobalt compound obtained in the step (1) with a cyclopentadiene monomer in a second alcoholic solvent to obtain a mixed solution containing cobaltocene, and carrying out distillation to remove the solvent to obtain a coarse product of cobaltocene; (3) dissolving the cobaltocene coarse product obtained in the step (2) into a non-proton solvent, filtering, adding an ether solvent into the condensed filtrate, and carrying out recrystallization to obtain cobaltocene solids. The raw materials used in the provided preparation technology all have a wide source and low price. The reagents, which need strict reaction conditions, such as metal sodium, amino sodium, and the like, are not used in the provided preparation technology. Moreover, the reaction conditions are mild, the operation is convenient and safe, the production cost is low, thus the preparation technology is very suitable for industrial production, and the cobaltocene product is high-purity solid crystals.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a preparation process of a metal compound cobaltocene. Background technique [0002] Dicyclopentadiene-cobalt, the English name is cobaltocene, dicyclopentadiene-cobalt or Bis(cyclopentadienyl)cobalt, the CAS registration number is 1277-43-6; the structural formula is as follows: [0003] [0004] Cobaltocene is mainly used as a catalyst for polymer polymerization, and more advanced research shows that cobaltocene is also used to catalyze the ring sum of substituted pyridines and the organic asymmetric synthesis reaction. The preparation method of cobalt dicene has the following reports at present: [0005] For example, the patent name is the preparation method of a catalyst for the synthesis of 2-picoline, and the method disclosed in the specification example of CN101108366A is: add tetrahydrofuran and sodium amide in a sodium salt kettle, and drop Add cyclopen...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F17/02
Inventor 赵长阔何芋岐王先恒高磊
Owner ZUNYI MEDICAL UNIVERSITY
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