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Method for regulating and controlling photocatalytic reduction reaction selectivity of unsaturated aldehyde ketone by utilizing solvent

A technology of reaction selectivity and solvent regulation, applied in chemical instruments and methods, reduction preparation of oxygen-containing functional groups, organic chemistry, etc., can solve problems such as difficult reaction control

Active Publication Date: 2020-10-02
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It is difficult to control the reaction due to the generation of more free radical active species during the reaction

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Add titanium dioxide (1g / L) and cinnamaldehyde (0.1mmol / L) into a double-layer glass reactor filled with 10mL of methanol, seal it and pass in argon (0.02MPa~0.1MPa) for 30min, and remove the reaction by bubbling. After the oxygen in the container and the solution is sealed, the reaction temperature is controlled by a water bath to 25 ° C, the stirring speed is 20 rpm, and then the 300W xenon lamp is used to intercept the light in the 360-720nm band for 1 hour to stop the reaction. The reaction product is mainly cinnamyl alcohol. , the selectivity of cinnamyl alcohol was 100%, and the yield of reductive hydrogenation was 64%.

Embodiment 2

[0029] Add titanium dioxide (1g / L) and cinnamaldehyde (0.1mmol / L) into a double-layer glass reactor with 10mL of methanol: acetonitrile = 1:1, seal it and let it flow with argon (0.02MPa~0.1MPa) for 30min After removing the oxygen in the reactor and the solution by bubbling, seal it, control the reaction temperature to 25°C through a water bath, and the stirring speed to 20 rpm, and then use a 300W xenon lamp to intercept light in the 360-720nm band for 1 hour to stop the reaction. The reaction products are mainly cinnamyl alcohol and phenylpropionaldehyde, the selectivity of cinnamyl alcohol is 100%, and the yield of reductive hydrogenation is 73%.

Embodiment 3

[0031] Add titanium dioxide (1g / L) and cinnamaldehyde (0.1mmol / L) into a double-layer glass reactor filled with 10mL of methanol: acetonitrile = 4:6, seal it and pass in argon (0.02MPa~0.1MPa) for 30min After removing the oxygen in the reactor and the solution by bubbling, seal it, control the reaction temperature to 25°C through a water bath, and the stirring speed to 20 rpm, and then use a 300W xenon lamp to intercept light in the 360-720nm band for 1 hour to stop the reaction. The reaction products are mainly cinnamyl alcohol and phenylpropanal, the selectivity of cinnamyl alcohol is 94%, and the yield of reductive hydrogenation is 82%.

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Abstract

The invention belongs to the technical field of photocatalytic reduction synthesis. The invention particularly relates to a method for regulating and controlling the photocatalytic reduction reactionselectivity of unsaturated aldehyde ketone by utilizing a solvent. The method comprises the following steps: adding a photocatalyst, unsaturated aldehyde ketone and a solvent into a reaction container, irradiating the reaction container with a light source under an anaerobic condition to react, and adjusting the proportion and / or type of alcohol in the reaction solvent to obtain reduction productswith different selectivity. The method is simple to operate, good in selectivity and high in yield, wherein the highest selectivity can reach 100% and the highest yield can reach 100%.

Description

technical field [0001] The invention belongs to the technical field of photocatalytic reduction synthesis, and in particular relates to a method for regulating the photocatalytic reduction reaction selectivity of unsaturated aldehydes and ketones by using a solvent. Background technique [0002] In industry, unsaturated alcohol compounds are often used in food flavors, spices and pharmaceutical intermediates, etc., and their conventional preparation methods are obtained by selective reduction of unsaturated aldehydes and ketones, but in fact, the C=C double bond is thermodynamically stronger than the C=C The O double bond is more easily reduced. In order to achieve selective reduction, the commonly used method is to support the synthesis of catalysts through noble metals, and under the conditions of heating and pressure, H 2 As a hydrogen source, this method requires harsh reaction conditions, high equipment requirements, and the use of loaded noble metals also increases th...

Claims

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Application Information

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IPC IPC(8): C07C29/14C07C33/32C07C45/69C07C47/228
CPCC07C29/14C07C45/69C07C33/32C07C47/228
Inventor 赵进才商锦婷马万红陈春城籍宏伟盛桦
Owner INST OF CHEM CHINESE ACAD OF SCI