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Catalyst for synthesizing piperidine nitroxide radical and preparation method thereof

A technology for the synthesis of nitroxide free radicals and piperidine, applied in chemical instruments and methods, physical/chemical process catalysts, organic chemistry, etc., can solve the problems of difficult catalyst reuse, long reaction time, complex process, etc., and achieve high yield High performance, good specificity and high catalytic efficiency

Inactive Publication Date: 2012-12-19
NANJING FORESTRY UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In summary, the shortcomings of the current synthesis of piperidine nitroxide free radicals are complex process, long reaction time, low yield, and difficulty in catalyst reuse.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0018] Example 1: Weigh 10g of NaOH solid to make a 1.0mol / L solution, then weigh 25.5g of MgCl 2 ·6H 2 O was made into a 1.0mol / L solution and added to the NaOH solution to form a white flocculent precipitate, and then 29.1g of diatomaceous earth was added to it, fully stirred at a speed of 1000rpm, filtered after 1h, and then washed with distilled water until there was no Cl - Until it exists, the obtained filter cake is placed in an electric drying oven, dried at 120°C for 24 hours, and then ground to obtain Mg(OH) 2 - diatomaceous earth catalyst.

example 2

[0019] Example 2: 14.1g tetramethylpiperidine is added in the four-necked round-bottomed flask, then 30ml methanol and 0.2g example 1 catalyst are added, the reaction temperature is controlled at 70°C with a constant temperature water bath, and the constant pressure dropping funnel is used for 1 hour. 28.3g 30%H 2 o 2 After the dropwise addition was completed, the reaction was continued for 1 h and then terminated. The yield of TEMPO prepared by this process is 97%, and there are no other by-products detected by gas chromatography.

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Abstract

The invention belongs to the technical field of organic synthesis catalysts and particularly relates to a preparation technology of a catalyst for synthesizing piperidine nitroxide radical. The aperture of kieselguhr is 3-16 microns and the aperture of Mg(OH)2 is 1.5-2 microns; under a condition of high-speed stirring, newly made Mg(OH)2 floccules are evenly adsorbed on the surface of the porous material kieselguhr to ensure that the specific surface area of effective catalysis of active ingredients is improved by hundreds of times. When the catalyst is used for synthesizing the piperidine nitroxide radical, the reaction speed is high, the specificity is good, the yield is high and the Mg(OH)2-kieselguhr compound catalyst can be repeatedly used 5 times without losing the activity. The yield of the piperidine nitroxide radical synthesized by using the catalyst is as high as 97% and no by-product is produced. The catalyst provided by the invention has low cost and good stability and is simple for operation, nontoxic, pollution-free and environment-friendly.

Description

1. Technical field: [0001] The invention relates to a catalyst for synthesizing piperidine nitroxide free radicals and a preparation method thereof. The invention greatly accelerates the synthesis reaction rate, reduces by-products and improves product yield, and the preparation process of the catalyst is simple and easy to operate. 2. Background technology: [0002] Piperidine nitroxide radicals are a new class of stable free radicals. Their extensive applications in theory and spin-labeling methods attract attention and become one of the main development directions of free radical chemistry. In the 1960s, there were reports on piperidine-like nitroxide free radicals. Its lone pair of electrons produces a delocalization effect between the nitrogen-oxygen bonds, making it a stable nitroxide free radical that can be stored for a long time. without deterioration. Since the 1960s, people have conducted in-depth research on nitroxide free radicals and put forward many innovati...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J21/16B01J21/10C07D211/94
Inventor 戴红旗袁洋春戴路孙旋万丽
Owner NANJING FORESTRY UNIV
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