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Method for synthesizing 2-methylpyridine organic cobalt catalyst

A technology of picoline and organic cobalt, which is applied in the field of synthesizing 2-picoline organic cobalt catalysts, can solve the problems of low crystal purity of organic cobalt catalysts, unsatisfactory catalytic effect, and large loss in step-by-step reactions. The effect of fast drying speed, increased yield, and improved purity

Pending Publication Date: 2020-08-25
ANHUI COSTAR BIOCHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main disadvantage of this method is that the operation steps are complicated, the stepwise reaction loss is relatively large, and the productive rate is not high.
Finally, the removal of metal salts such as sodium chloride is not clean, and the purity of the organic cobalt catalyst crystal obtained is not high, and the catalytic effect is not ideal.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 1. Synthesis. Put 89g of cobalt chloride hexahydrate, 40g of sodium carbonate and 33g of cyclopentadiene into a 1000mL reaction flask, add 500mL of N,N-dimethylformamide solution, stir to dissolve, set the temperature at 90°C, and reflux for 10h .

[0025] 2. Processing. The resulting reaction solution was cooled, and distilled under reduced pressure at 80°C to distill off the solvent N,N-dimethylformamide to obtain a pink solid, which was extracted by adding 200 mL of water and 200 mL of dichloromethane to release an aqueous solution. Repeat the operation three times, then add sodium sulfate aqueous solution to extract once, and release the aqueous solution. The obtained dichloromethane solution containing the organic cobalt catalyst was crystallized at -5°C, and after refrigerated for 8 hours, the reaction solution was taken out and solids precipitated out. The organic cobalt catalyst crystals were obtained by suction filtration. Dry the crystal at 50°C, weigh 40g...

Embodiment 2

[0027] 1. Synthesis. Put 107g of cobalt chloride hexahydrate, 48g of sodium carbonate and 33g of cyclopentadiene into a 1000mL reaction flask, add 800mL of N,N-dimethylformamide solution, stir to dissolve, set the temperature at 93°C, and reflux for 8h .

[0028] 2. Processing. The resulting reaction solution was cooled, and distilled under reduced pressure at 80°C to distill off the solvent N,N-dimethylformamide to obtain a pink solid, which was extracted by adding 200 mL of water and 200 mL of dichloromethane to release an aqueous solution. Repeat the operation three times, then add sodium sulfate aqueous solution to extract once, and release the aqueous solution. The obtained dichloromethane solution containing the organic cobalt catalyst was crystallized at -5°C, and after refrigerated for 8 hours, the reaction solution was taken out and solids precipitated out. The organic cobalt catalyst crystals were obtained by suction filtration. Dry the crystal at 50°C, weigh 42g...

Embodiment 3

[0030] 1. Synthesis. Put 109g of cobalt chloride hexahydrate, 49g of sodium carbonate and 50g of cyclopentadiene into a 1000mL reaction flask, add 700mL of N,N-dimethylformamide solution, stir to dissolve, set the temperature at 95°C, and reflux for 10h .

[0031] 2. Processing. The resulting reaction solution was cooled, and distilled under reduced pressure at 80°C to distill off the solvent N,N-dimethylformamide to obtain a pink solid, which was extracted by adding 200 mL of water and 200 mL of dichloromethane to release an aqueous solution. Repeat the operation three times, then add sodium sulfate aqueous solution to extract once, and release the aqueous solution. The obtained dichloromethane solution containing the organic cobalt catalyst was crystallized at -5°C, and after refrigerated for 8 hours, the reaction solution was taken out and solids precipitated out. The organic cobalt catalyst crystals were obtained by suction filtration. The crystals were dried at 50°C, ...

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Abstract

The invention discloses a method for synthesizing a 2-methylpyridine organic cobalt catalyst, which comprises the following steps: step 1, selecting sodium carbonate as alkali, putting cobalt chloride, cyclopentadiene and sodium carbonate into N, N-dimethylformamide for high-temperature reaction, and enabling cyclopentadiene to be coordinated with cobalt chloride under an alkaline condition to generate an organic cobalt catalyst; 2, dissolving the generated organic cobalt catalyst in N, N-dimethylformamide, evaporating N, N-dimethylformamide through reduced pressure distillation, adding waterand dichloromethane, dissolving sodium chloride in water, separating after layering, repeatedly extracting to reduce the salt content in the organic solvent, putting the obtained dichloromethane solution in a low-temperature environment, slowly precipitating the organic cobalt catalyst, carrying out suction filtration on the precipitated crystal, and drying the crystal to obtain the high-purity organic cobalt catalyst. The required organic cobalt catalyst is obtained through one-step reaction, and the purity of a final product can be improved through a crystallization method.

Description

technical field [0001] The invention relates to a method for synthesizing a catalyst, in particular to a method for synthesizing a 2-picoline organic cobalt catalyst. Background technique [0002] 2-Methylpyridine, also known as α-Methylpyridine, is mainly used to prepare 2-vinylpyridine and 2-methyl-5-vinylpyridine as raw materials for dipping butylpyridine latex for rubber skeleton materials; it can also be used for Preparation of nitrogen fertilizer synergist (N-Serve), livestock deworming drug, poultry drug, film sensitizer additive, dye intermediate and rubber accelerator, etc.; used as an experimental reagent for the determination of cobalt, cyanate and iron ; In medicine, it is used to prepare drugs such as scarni, chlorpheniramine, pralidoxime, acetylcysteine, and long-acting sulfonamide; in pesticides, it uses 2-methylpyridine as a raw material to synthesize an important pesticide intermediate 2 -Hydroxy-3,5,6-trichloropyridine, 2-trifluoromethyl-6-chloropyridine, ...

Claims

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Application Information

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IPC IPC(8): B01J31/22C07F17/02C07D213/16
CPCB01J31/2295C07F17/02C07D213/16B01J2531/845
Inventor 韦琛鸿宋利刚刘典典刘皇见王婕王丹
Owner ANHUI COSTAR BIOCHEM CO LTD
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