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A kind of magnetic resolving agent and preparation method thereof

A resolving agent and magnetic technology, applied in organic chemical methods, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of limited large-scale application, difficulty in recycling, poor recyclability, etc., and achieve good resolution. Effect, high utilization rate, convenient recycling effect

Inactive Publication Date: 2018-11-06
JILIN INST OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the chiral (Salen)-Co complex is difficult to separate from the product and difficult to recycle, which limits its large-scale application.
[0004] In the prior art, this separation problem is solved by immobilizing the chiral (Salen)-Co complex. The commonly used immobilization methods include immobilizing the chiral (Salen) -Co complexes are immobilized on polymers or inorganic supports. Although these methods can realize the immobilization of complexes, they generally have the disadvantages of easy deactivation of catalysts during hydrolysis and resolution, and poor recyclability.

Method used

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  • A kind of magnetic resolving agent and preparation method thereof
  • A kind of magnetic resolving agent and preparation method thereof
  • A kind of magnetic resolving agent and preparation method thereof

Examples

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preparation example Construction

[0032] The present invention provides a kind of preparation method of resolving agent described in above-mentioned scheme, comprises the following steps:

[0033] Will Fe 3 o 4 Particles, silicon source and solvent are mixed, and the reaction is carried out under the condition of pH value of 9-10 to obtain Fe 3 o 4 @SiO 2 Composite magnetic particles;

[0034] the Fe 3 o 4 @SiO 2 Composite magnetic particles, acid-binding agent, benzene and chiral Salen-Co(Ⅲ) complex were mixed for Friedel-Crafts alkylation reaction to obtain magnetic Fe 3 o 4 @SiO 2 @Salen-Co(Ⅲ) resolving agent.

[0035] The present invention will Fe 3 o 4 Particles, silicon source and solvent are mixed, and the reaction is carried out under the condition of pH value of 9-10 to obtain Fe 3 o 4 @SiO 2 Composite magnetic particles. In the present invention, the Fe 3 o 4 The particle size of the particles is consistent with the particle size of the above-mentioned core, and will not be repeated...

Embodiment 1

[0074] Weigh 6 grams of FeCl 2 4H 2 O (0.003mol), 16 grams of FeCl 3 ·6H 2 O (0.01mol) and 0.444 grams of sodium dodecylbenzene sulfate are added to a 300ml mixed solution of ethanol and water, the alcohol-water ratio of the mixed solution is 5:1; the above solution is injected into a three-necked flask, connected to a mechanical stirrer, And connect the catheter, and start to feed nitrogen at the same time, so that the reaction is in an oxygen-free environment;

[0075] Set the temperature of the water bath to 45°C and start stirring. The solution in the flask begins to heat up gradually. After the temperature reaches the temperature, start to add 60ml of ammonia water to the solution, and control the pH value of the reaction solution to 7-10. It can be observed that the solution changes from orange to yellow to reddish-brown and finally to black;

[0076] After the addition of ammonia water is completed, continue to stir at constant temperature for 45 minutes to make it ...

Embodiment 2

[0083] Weigh 15.66g (0.1mol) of 5-chlorosalicylaldehyde and dissolve it in 100ml of absolute ethanol, add the prepared solution into a three-necked flask, connect to mechanical stirring, and protect with nitrogen;

[0084] Weigh 5.71g (0.05mol) (1R,2R)-(-)-1,2-cyclohexanediamine, add it dropwise to the above mixture with a dropping funnel, after the dropwise addition is completed, heat to reflux, and control the reaction temperature to 78°C, react for 2 hours to obtain the Salen ligand;

[0085] After the above reaction is completed, 12.45g (0.05mol) Co(OAc) 2 4H 2 O was dissolved in 60ml of absolute ethanol, and was directly added dropwise into the reaction solution of the Salen ligand. 2 Under protection, reflux reaction at a temperature of 78°C for 2 hours to obtain a Salen-Co(II) complex;

[0086] Add 2.12g (0.05mol) LiCl to the above reaction solution, and blow air into it with an air compressor at the same time, reflux the reaction at a temperature of 77°C for 1h, sto...

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Abstract

The invention provides a magnetic resolving agent, and a preparation method thereof. The preparation method comprises following steps: Fe3O4 is prepared firstly, surface modification of Fe3O4 nanoparticle is carried out so as to obtain Fe3O4@SiO2 composite magnetic particle, Friedel Crafts alkylation with chiral Salen-Co (III) catalyst is carried out so as to obtain the magnetic Fe3O4@SiO2@Salen-Co(III) resolving agent. According to the preparation method, surface modification of Fe3O4 is carried out, so that the surface of Fe3O4@SiO2 composite magnetic particle is provided with a large amount of hydroxyl, and Friedel Crafts alkylation is adopted for high efficiency firm loading of Salen-Co(III) ligand. When the Fe3o4@SiO2@Salen-Co(III) resolving agent is applied to hydrolytic resolution of racemic epoxy chloropropane, resolution effect is excellent, recycling is convenient to realize, and recycling performance is excellent.

Description

technical field [0001] The invention relates to the technical field of magnetic complexes, in particular to a magnetic resolving agent and a preparation method thereof. Background technique [0002] Epichlorohydrin, chemical name is 1-chloro-2,3-epoxypropane, molecular formula C 3 h 5 OCl is a volatile and unstable colorless liquid with a pungent odor similar to chloroform and ether, toxic and narcotic. Racemic epichlorohydrin is a widely used chemical raw material with low price . Chiral epichlorohydrin is a very important raw material for organic synthesis. By using chiral epichlorohydrin as a reaction starting material, many pharmaceutical intermediates with high optical purity can be prepared, which can be used in the fields of medicine, pesticides, chemicals, materials, etc. widely. Chiral epichlorohydrin is expensive and is generally obtained by splitting the racemate chemical epichlorohydrin. [0003] In the prior art, the commonly used method for splitting racem...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/22C07D303/08
CPCB01J31/2217B01J2531/0261B01J2531/845C07B2200/07C07D303/08
Inventor 计海峰郑娣莲戴传波王卫东刘放
Owner JILIN INST OF CHEM TECH
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