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Preparation of a natural feather-supported Pd catalyst and its application in the synthesis of pyrimidines

A compound and catalyst technology, applied in the application field of the catalyst in synthesizing pyrimidine compounds, can solve the problems such as the catalyst cannot be reused, the environmental threat, the product is difficult to be separated, etc., and achieve high catalytic activity and stability, low-cost carrier, Prepare simple effects

Inactive Publication Date: 2019-07-02
NORTHWEST UNIVERSITY FOR NATIONALITIES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, most of the coupling reactions involving pyrimidine compounds are carried out in a homogeneous system of transition metals. After the reaction, the products are difficult to separate and the catalyst cannot be reused, which poses a great threat to the environment.

Method used

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  • Preparation of a natural feather-supported Pd catalyst and its application in the synthesis of pyrimidines
  • Preparation of a natural feather-supported Pd catalyst and its application in the synthesis of pyrimidines
  • Preparation of a natural feather-supported Pd catalyst and its application in the synthesis of pyrimidines

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Embodiment 1, preparation of natural chicken feather supported Pd catalyst

[0045] Take 0.5-1.0 g of natural chicken feathers, wash them with detergent, cut them into pieces, soak them in ethanol solution, reflux at 90°C for 24 h, and dry them to obtain the natural chicken feather catalyst carrier.

[0046] At room temperature, 0.2~0.3 g Pd(OAc) 2 Add 40~50 mL deionized water to get Pd(OAc) 2 solution; take 0.5-1.0 g of the natural chicken feather catalyst carrier obtained above and soak it in Pd(OAc) 2 After 2~3 h in the solution, the natural chicken feathers changed from white to brown-yellow, and the turbid brown-yellow solution turned into a light yellow to colorless transparent solution; filtered, washed, and dried to obtain the natural chicken feather-loaded Pd catalyst—natural chicken Feather-Pd(OAc) 2 . In the catalyst, the Pd content is 0.10-0.15mmol / g.

Embodiment 2

[0047] Embodiment 2, the synthesis of typical dihydropyrimidine compounds

[0048] (1) Preparation of pyrimidinethione

[0049] Take ethyl acetoacetate (13.0 g, 100 mmol), 4-methoxybenzaldehyde (10.6 g, 100 mmol), thiourea (9.1 g, 120 mmol) into a 250 mL round bottom flask, and add 80 mL Absolute ethanol; add 0.5 mL of concentrated sulfuric acid dropwise under stirring, heat up to 80°C, reflux for 8 hours, and a white precipitate precipitates; pour it into water after cooling, filter with suction, wash the filter cake with hot water, collect the filter cake, and weigh it with ethanol Crystallization gave 4-methoxy substituted pyrimidinethione. The reaction formula is as follows:

[0050]

[0051] (2) Preparation of pyrimidine sulfide

[0052] Take the above-mentioned 4-methoxy substituted pyrimidinethione (1.0mmol), phenylboronic acid (3.0 mmol), o-phenanthroline (2.0mmol), Cu(OAc) 2 (1.0 mmol), 4Ǻ molecular sieve powder (750 mg) and 1,2-dichloroethane (15 mL) were add...

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Abstract

The invention provides a method for preparing natural feathers to load a Pd catalyst. The natural feathers are washed, cut into pieces, soaked in ethanol, refluxed, and dried to obtain a natural feather catalyst carrier; and then the natural feather carrier is dispersed in palladium. Soak in the aqueous solution of salt for 1 to 2 hours, filter, wash, and dry to obtain a natural feather-loaded Pd catalyst. This catalyst has high selectivity for products in the synthesis of pyrimidine compounds and has a high yield. In addition, the natural feather carrier of the present invention is cheap, non-toxic, and easy to obtain, and the catalyst is simple to prepare, and the catalyst can be recycled without activation treatment, which is in line with the concept of green chemistry.

Description

technical field [0001] The invention relates to the preparation of a supported Pd catalyst, in particular to the preparation of a Pd catalyst supported by natural feathers, and also relates to the application of the catalyst in the synthesis of pyrimidine compounds. Background technique [0002] Today, when environmental issues are of great concern, with the strict requirements for clean synthesis in pharmaceutical synthetic chemistry, fine organic synthetic chemistry, and combinatorial chemistry, the development of recyclable supported heterogeneous catalysts has become a key goal for chemists to solve the above problems. One of the main strategies. In homogeneous catalysis, transition metal (Ru, Rh, Pd, Cu, etc.) catalyzed coupling reactions show good catalytic activity and are tolerant to many functional groups, so they are widely used in coupling reactions. However, the price of transition metals is too expensive, and the catalysts are not easy to recycle, cannot be reu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J35/06B01J31/04B01J31/22B01J31/24B01J31/30C07D471/04
CPCC07D471/04B01J31/04B01J31/2213B01J31/2409B01J31/30B01J2531/0238B01J2531/824B01J35/58
Inventor 吴尚王彦斌苏琼杨全录张宏苑沛霖尹奋平贺媛王明明杜秀芳张银潘
Owner NORTHWEST UNIVERSITY FOR NATIONALITIES
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