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Supported Pd catalyst and application thereof

A catalyst, supported technology, used in molecular sieve catalysts, physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, etc., can solve problems such as poor selectivity, suppress side reactions, and improve selectivity. , the effect of a wide range of applications

Active Publication Date: 2014-08-06
ZHANGJIAGANG IND TECH RES INST CO LTD DALIAN INST OF CHEM PHYSICS CHINESE ACADEMY OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The currently widely used porous silica or Pd catalysts supported by carbon materials still show relatively poor selectivity in this type of reaction.

Method used

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  • Supported Pd catalyst and application thereof
  • Supported Pd catalyst and application thereof
  • Supported Pd catalyst and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] K 2 CO 3 Modified mesoporous silica-based foam-supported palladium catalyst (K 2 CO 3 -Pd / MCF) preparation:

[0030] Weigh 53mg Pd(NH 3 ) 4 Cl 2 ·H 2 O solid, be dissolved in 40ml deionized aqueous solution, then add 100l concentrated ammonia water to make system pH=11. Add 800 mg of mesoporous silicon-based foam (MCF) to the above Pd precursor solution and stir at room temperature for 6 hours to make the Pd 2+ Can be completely adsorbed to the surface of the carrier. After the adsorption equilibrium was reached, the mixture was centrifuged at a high speed to separate the solid from the liquid, the supernatant was discarded, and the lower solid was washed with deionized water and ethanol several times, and then dried in a drying oven at 80°C for 12 hours. The dried adsorbed Pd 2+ Put the solid into the catalyst treatment device, and use H under the condition of 300°C 2 After reduction for 3 hours, the Pd catalyst supported by mesoporous silicon-based foam (Pd / M...

Embodiment 2

[0032] In addition to using 0.5mol / l Na 2 CO 3 solution, prepared in the same manner as described in Example 1, to obtain Na 2 CO 3 Modified Pd / MCF (Na 2 CO 3 -Pd / MCF).

Embodiment 3

[0034] In addition to using 0.5mol / l K 3 PO 4 solution, prepared in the same manner as described in Example 1, to obtain K 3 PO 4 Modified Pd / MCF (K 3 PO 4 -Pd / MCF).

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Abstract

The invention relates to a supported Pd catalyst and application thereof to racemization and dynamic kinetic resolution of amine compounds. The supported Pd catalyst shows high catalytic activity and product selectivity more than 97% when being applied to racemization reaction of (S)-1-phenylethylamine. When the Pd catalyst is applied to dynamic kinetic resolution of 1-phenylethylamine, the yield of a target amide reaches 95% or more. According to the technical scheme, the application scope of the catalyst for racemization and dynamic kinetic resolution of amine compounds is substantially expanded. The preparation method of the catalyst is simple, environment-friendly and wide in application scope.

Description

technical field [0001] The invention relates to a supported Pd catalyst, a preparation method thereof and the application of the catalyst in racemization and dynamic kinetic resolution of amine compounds. Background technique [0002] Chiral amines are important intermediates in organic synthesis, and are often used as basic units to prepare various physiologically active compounds, which are widely used in pharmaceutical, agrochemical and other fields. There are two main physical methods for the preparation of chiral amines, diastereomeric recrystallization and chiral chromatographic separation. Chemical methods are also divided into two categories, one is asymmetric hydrogenation of imines, enamines, oximes, etc., and the other is kinetic resolution (kinetic resolution, KR) of racemates, in which enzyme-catalyzed acylation resolution It is widely used because of its simple operation, mild conditions and high selectivity. However, the highest yield of chiral amines prepar...

Claims

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Application Information

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IPC IPC(8): B01J27/232B01J27/185B01J31/04B01J23/58B01J29/035C07C209/82C07C209/88C07C211/27
Inventor 李灿金倩茹张艳梅李军蒋宗轩
Owner ZHANGJIAGANG IND TECH RES INST CO LTD DALIAN INST OF CHEM PHYSICS CHINESE ACADEMY OF SCI
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