Carboxymethyl-beta-cyclodextrin intercalated water talc used for chiral resolution racemic modification and its preparation method

A racemate, chiral separation technology, applied in the direction of organic racemization, organic chemical methods, chemical instruments and methods, etc., can solve the problems of expensive columns, narrow application range, low performance, etc., to achieve easy reaction. , low cost, simple process effect

Inactive Publication Date: 2006-09-13
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chiral stationary phase high-performance liquid chromatography is the most widely used one, and its main disadvantages are: the column is expensive, and its performance is often lower than t

Method used

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  • Carboxymethyl-beta-cyclodextrin intercalated water talc used for chiral resolution racemic modification and its preparation method
  • Carboxymethyl-beta-cyclodextrin intercalated water talc used for chiral resolution racemic modification and its preparation method
  • Carboxymethyl-beta-cyclodextrin intercalated water talc used for chiral resolution racemic modification and its preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Step A: take by weighing 35.6g Zn(NO 3 ) 2 ·6H 2 O, 22.6g Al(NO 3 ) 3 9H 2 O and 9.06g NaNO 3 Dissolve in 200ml to remove CO 2 Mixed salt solution was prepared with water, another 11.2g NaOH was dissolved in 100ml to remove CO 2 Prepare alkaline solution in water, N at room temperature 2 Protection Use the double-drop method to slowly add the salt solution and alkali solution into the four-necked flask, and stir vigorously. Adjust the pH value to 7 with 0.1mol / L NaOH solution. The resulting slurry was crystallized at 70°C for 24 hours, and the product was centrifugally washed until neutral; the sample was taken out and dried at 70°C for 20 hours for characterization, and Zn 2 Al-NO 3 LDHs, whose Zn 2+ / Al 3+ =2.

[0028] Step B: 20.6 g of the sodium salt of carboxymethyl-β-cyclodextrin [C42 h 70-n o 35 ·(C 2 h 2 o 2 Na) n ] The solid was added into the four-neck flask containing the hydrotalcite precursor, N 2 Protected and heated to 70°C, reacted f...

Embodiment 2

[0032] Step A: take by weighing 30.7g Mg(NO 3 ) 2 ·6H 2 O and 22.6g Al(NO 3 ) 3 9H 2 O dissolved in 200ml to remove CO 2 Mixed salt solution was prepared with water, another 11.2g NaOH was dissolved in 100ml to remove CO 2 Prepare alkaline solution in water, N at room temperature 2 The salt solution and the alkali solution were slowly added into the four-necked flask by the double drop method, and the pH value was adjusted to 10 with 0.1mol / L NaOH solution after the dripping, and the resulting slurry was crystallized at 70°C for 24 hours, and the product was centrifugally washed until neutral; A small amount of sample was taken out and dried at 70°C for 20 hours for characterization, and Mg 2 Al-NO 3 LDHs, its Mg 2+ / Al 3+ =2.

[0033] Step B: According to the method similar to Step B in Example 1, the sodium salt of 20.6g carboxymethyl-β-cyclodextrin [C 42 h 70-n o 35 ·(C 2 h 2 o 2 Na) n ] The solid was added into the four-neck flask containing the sample, ...

Embodiment 3

[0037] Step A: Weigh 16.4g ZnCl 2 and 14.5g AlCl 3 ·6H 2 O dissolved in 200ml to remove CO 2 Mixed salt solution was prepared with water, another 11.2g NaOH was dissolved in 100ml to remove CO 2 Prepare alkaline solution in water, N at room temperature 2 The salt solution and the alkali solution were slowly added into the four-neck flask by the double-drop method, and the pH value was adjusted to 6 with 0.1mol / L NaOH solution after the dripping, and the obtained slurry was crystallized at 70°C for 24 hours, and the product was centrifugally washed until neutral; A small amount of samples were taken out and dried at 70°C for 20 hours for characterization, and Zn 2 Al-Cl LDHs, its Zn 2+ / Al 3+ =2.

[0038] Step B: According to the method similar to Step B in Example 1, the sodium salt of 20.6g carboxymethyl-β-cyclodextrin [C 42 h 70-n o 35 ·(C 2 h 2 o 2 Na) n ] The solid was added into the four-neck flask containing the sample, N 2 Protected and heated to 70°C for...

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Abstract

A carboxymethyl-beta-cyclodextin intercalated hydrotalcite for chiral resolving raceme is prepared through using LDHs as template to insert the carboxymethyl-beta- cyclodextrin anions in between the layers of hydrotalcite by ion change. Its chemical formula is also disclosed.

Description

[0001] Field [0002] The invention belongs to the field of chiral resolution of racemates, and in particular provides a carboxymethyl-β-cyclodextrin intercalated hydrotalcite for chiral resolution of racemates and a preparation method thereof. Background technique [0003] Mirror compounds that have the same chemical composition and molecular formula but have different orientations in space of the atoms or groups of atoms that make up the compound are called enantiomers. Because they cannot overlap each other like two human hands, they are also called chiral compounds. The different roles of enantiomers in biological processes, especially in the field of medicine, are increasingly recognized. In organisms, biomacromolecules are in a highly complex chiral environment, and enantiomer drugs will have significant differences in pharmacological activity, metabolic process and metabolites, and toxic and side effects when they enter the organism. Under normal circumstances, only o...

Claims

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Application Information

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IPC IPC(8): C01G1/00C07B57/00
Inventor 段雪卫敏刘晓磊路艳罗何静
Owner BEIJING UNIV OF CHEM TECH
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