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Debenzylation catalyst and preparation method thereof

A debenzylation catalyst and reducing agent technology, applied in the field of organic functional group chemistry, can solve the problems of reducing palladium loading, unstable loading of palladium microcrystals, loss of palladium microcrystals, etc.

Active Publication Date: 2021-09-14
山东华素制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this preparation method also has the problem of unstable loading of palladium microcrystals. After repeated use, palladium crystallites with unstable surfaces are easy to lose into the solution, thereby reducing the palladium loading.

Method used

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  • Debenzylation catalyst and preparation method thereof
  • Debenzylation catalyst and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0034] 0.089gPdCl 2 and 0.029g of 1,3-acetone dicarboxylic acid (CAS: 542-05-2) were dissolved in 1mL of 37% concentrated hydrochloric acid, 3mL of deionized water was added, and stirred to mix evenly to obtain a palladium precursor solution.

[0035] 10g of carboxyl multi-walled carbon nanotubes (diameter≤8nm; -COOH content of 3.86wt%; model CNT302, purchased from Beijing Deke Daojin Technology Co., Ltd.) were dispersed in 50mL of ethylene glycol aqueous solution (the volume of ethylene glycol and water ratio of 9:1), the carboxyl multi-walled carbon nanotube dispersion was obtained. In a water bath at 60°C, under stirring conditions, the palladium precursor solution was added dropwise to the carboxyl multi-walled carbon nanotube dispersion, and sodium hydroxide solution was added dropwise at the same time, the pH value of the reaction system was maintained at 9-10, and the reaction was kept for 24 hours. After the reaction is completed, wash with absolute ethanol and deioni...

Embodiment 2

[0037] 0.089gPdCl 2 and 0.044g of 1,3-acetone dicarboxylic acid (CAS: 542-05-2) were dissolved in 1mL of 37% concentrated hydrochloric acid, 5mL of deionized water was added, and stirred to mix evenly to obtain a palladium precursor solution.

[0038] 10g of carboxyl multi-walled carbon nanotubes (diameter≤8nm; -COOH content of 3.86wt%; model CNT302, purchased from Beijing Deke Daojin Technology Co., Ltd.) were dispersed in 50mL of ethylene glycol aqueous solution (the volume of ethylene glycol and water In the ratio of 8:2), the carboxyl multi-walled carbon nanotube dispersion was obtained. In a water bath at 50° C. under stirring conditions, the palladium precursor solution was added dropwise to the carboxy multi-walled carbon nanotube dispersion, and sodium hydroxide solution was added dropwise at the same time, the pH value of the reaction system was maintained at 9-10, and the reaction was kept for 24 hours. After the reaction is completed, wash with absolute ethanol and...

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Abstract

The invention discloses a debenzylation catalyst and a preparation method thereof. The preparation method comprises the steps of dropwise adding a palladium precursor solution into a carboxyl multi-walled carbon nanotube dispersion liquid at the temperature of 40-80 DEG C under a stirring condition, maintaining the pH value of a reaction system to be 9-10, and carrying out a heat preservation reaction to obtain the debenzylation catalyst. The catalyst not only is more stable in palladium microcrystal loading, but also is mainly distributed on the surface of the carbon nanotube, so that the actual loading amount and debenzylation conversion rate of the debenzylation catalyst Pd after repeated use can still be kept at a high level.

Description

technical field [0001] The invention belongs to the technical field of organic functional group chemistry, and in particular relates to a debenzylation catalyst and a preparation method thereof. Background technique [0002] The protection and deprotection of functional groups in the synthesis of organic compounds and natural products is an important research area of ​​functional group chemistry. [0003] As the functional group for protecting the amino group, including but not limited to, benzyl (Bn), p-nitrobenzyl (PNB), p-methoxybenzyl (PMB) and benzyloxycarbonyl (Cbz), 9-fluorenylmethoxycarbonyl ( Fmoc), allyloxycarbonyl (Alloc), tert-butoxycarbonyl (Boc), p-methoxybenzyloxycarbonyl (PMZ), etc. Benzyl is one of the most commonly used functional groups, introduced under basic conditions by suitable halides. The removal of benzyl groups is also relatively easy, and can be removed by catalytic hydrogenolysis, liquid ammonia and sodium or lithium, oxidative debenzylation, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22
CPCB01J31/223B01J2531/824Y02P20/55
Inventor 王熙红滕世涛郑海轩林丽丽
Owner 山东华素制药有限公司