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Supported catalyst, as well as preparation method and application thereof in synthesis of 3,4-dihydropyrimidine-2-ketone

A technology of supporting catalysts and carriers, applied in chemical instruments and methods, physical/chemical process catalysts, organic chemistry, etc., can solve the problems of yellowish color of crude products, large product loss, and increased cost, so as to simplify operations and improve products. Yield and production cost reduction effects

Inactive Publication Date: 2012-10-10
SHANGHAI INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the color of the crude product obtained by synthesis is yellow, and the purity is not high. It must be recrystallized to obtain a product with higher purity.
Moreover, although the recrystallization improves the product purity, the product loss is relatively large, and the cost is increased and the operation is complicated.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] A supported catalyst, which uses 20-40 mesh granular activated carbon as a carrier, and is made by repeatedly adsorbing copper chloride on 20-40 mesh granular activated carbon, wherein the supported copper chloride is calculated by mass percentage, that is, granular activated carbon: chloride Copper is 95%: 5%.

[0020] The preparation method of above-mentioned a kind of loaded catalyst specifically comprises the following steps:

[0021] (1) Weigh 50g of 20~40mesh granular activated carbon, soak it with 0.5% hydrochloric acid for 3 hours, then wash it with deionized water until it is neutral, and after vacuum filtration, the obtained filter cake is at 120 Dry at ℃;

[0022] (2) Soak the activated carbon obtained after drying in step (1) in an aqueous solution of copper chloride with a concentration of 30% by mass for 5-10 hours, and vacuum filter the obtained filter cake under the environment of 120°C drying;

[0023] (3), soak the activated carbon dried in step (2)...

Embodiment 2

[0029] A supported catalyst, which uses activated carbon with 20-40 mesh particles as the carrier, and is made by adsorbing copper chloride on the granular activated carbon for many times, wherein the supported copper chloride is calculated by mass percentage, that is, granular activated carbon: copper chloride is 90 %: 10%.

[0030]

[0031] The preparation method of above-mentioned a kind of loaded catalyst specifically comprises the following steps:

[0032] (1) Weigh 50g of 20-40 mesh granular activated carbon, soak it with 1.0% hydrochloric acid by mass percentage for 4 hours, then wash it with deionized water until neutral, vacuum filter it, and put it under the environment of 140℃ drying;

[0033] (2) Soak the activated carbon dried in step (1) in a copper chloride solution with a mass percentage concentration of 50% for 5-10 hours, and then dry it at 140°C after vacuum filtration;

[0034] (3), soak the activated carbon dried in step (2) and adsorbed copper chloride...

Embodiment 3

[0040] A supported catalyst, that is, activated carbon with 20-40 mesh particles as the carrier, and the granular activated carbon is adsorbed copper chloride four times, and the supported copper chloride is calculated by mass percentage, that is, granular activated carbon: copper chloride is 85%: 15%.

[0041] The preparation method of above-mentioned a kind of loaded catalyst specifically comprises the following steps:

[0042] (1) Weigh 50g of 20~40mesh granular activated carbon, soak it with 0.5% hydrochloric acid for 5 hours, then wash it with deionized water until neutral, vacuum filter it, and put it under the environment of 120℃ drying;

[0043] (2) Soak the activated carbon obtained after drying in step (1) in a copper chloride solution with a mass percent concentration of 50% for 5-10 hours, and dry it at 150°C after vacuum filtration;

[0044] (3), soak the activated carbon dried in step (2) and adsorbed cupric chloride in a cupric chloride solution with a mass pe...

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Abstract

The invention discloses a supported catalyst, as well as a preparation method and an application of the supported catalyst in synthesis of 3,4-dihydropyrimidine-2-ketone. The supported catalyst takes granular active carbon as a carrier and is formed by absorbing copper chloride; and the loaded and absorbed copper chloride is calculated by mass percent, i.e., the ratio between the granular active carbon and the copper chloride is (85-95%):(15-5%). The supported catalyst is used for the synthetic reaction for preparing the 3,4-dihydropyrimidine-2-ketone so as to enable the synthetic reaction and purification to be completed in one step, thus not only improving the product yield, but also simplifying the operation; and therefore, the production cost is reduced. Finally, the obtained 3,4-dihydropyrimidine-2-ketone is good in color and luster as well as high in purity.

Description

Technical field [0001] The invention involves a load catalyst and its preparation method and the application in the synthesis of 3,4-dihydrial-2-ketone synthesis, that is, loaded on the activated carbon with Louisic acid, as preparation of 3,4-dihydridine-2-The catalyst used for ketone synthesis reactions is more specifically involved in the catalysts used for 3,4-dihydrial-2-ketone synthesis reactions. Background technique [0002] 3,4-dihydrial-2-ketone is a drug intermediate with antiviral, antitumor and antibacterial and anti-inflammatory effects, and also has the effects of regulating and lowering blood pressure.Anti -cancer, sterilization and other fields have broad prospects.Therefore, the synthesis of such compounds in recent years has caused great interest.People use various synthesis methods to increase the income of 3,4-dihydrine-2-ketones.However, the color obtained by the synthetic product is yellow and the purity is not high. It must be heavy crystals to obtain prod...

Claims

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Application Information

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IPC IPC(8): B01J27/122C07D239/22
Inventor 王红高永红金东元
Owner SHANGHAI INST OF TECH
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