A method for preparing anisaldehyde by catalytic liquid phase selective oxidation

A technology of phase selection and anisaldehyde, applied in chemical instruments and methods, preparation of carbon-based compounds, preparation of organic compounds, etc., can solve the problems of high cost of anisaldehyde, corrosion of equipment, large consumption of raw materials, etc., and achieve conversion rate of raw materials and The effect of high product selectivity and mild reaction conditions

Active Publication Date: 2022-06-03
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Application Information

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Problems solved by technology

[0004] In order to solve the high cost of preparing anisaldehyde from raw materials such as anethole and p-hydroxybenzaldehyde; the preparation of anisaldehyde from phenol has a long route, serious equipment corrosion, a large amount of acidic waste water is produced, and the environment is greatly affected; The reaction temperature of aldehyde is high, excessive oxidation is easy to occur, the consumption of raw materials is large, and the product selectivity is low. This application provides a method for the production of anisaldehyde by catalytic liquid phase selective oxidation. , a method for preparing anisaldehyde by catalytic liquid-phase selective oxidation of p-methoxytoluene, which has the advantages of mild reaction conditions, high conversion rate of raw materials and high product selectivity, and recyclable catalyst.

Method used

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  • A method for preparing anisaldehyde by catalytic liquid phase selective oxidation
  • A method for preparing anisaldehyde by catalytic liquid phase selective oxidation
  • A method for preparing anisaldehyde by catalytic liquid phase selective oxidation

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Dissolve 1 g of hydrated cobalt acetate in 100 ml of methanol, add 100 ml of methanol dissolved in 2 g of benzotriazole under stirring, continue to stir for 2 h, filter, wash the obtained solid with methanol, dry in the air, and roast at 700 °C for 4 h under nitrogen protection. Soak in 10% dilute hydrochloric acid for 8 h, filter and wash with water until neutral, and the obtained solid was vacuum dried at 80 °C for 8 h to obtain 1 g of nitrogen-doped carbon-supported cobalt catalyst (Co@N-C).

[0032] Take 20mg of the obtained catalyst (Co@N-C) and add it to the 50mL reactor containing 2g p-methoxytoluene and 8g 1,1,1,3,3,3-hexafluoro-2-propanol, stir, and heat up. to 80°C, charged with oxygen to a pressure of 0.4MPa, reacted for 8h, and qualitatively and quantitatively analyzed the reaction product by gas chromatography-mass spectrometry. The conversion rate of p-methoxytoluene was 70%, and the selectivity of anisaldehyde was 90%. .

Embodiment 2～3

[0034] In Examples 2-3, the effects of different metals on the reaction were studied, and the specific method was similar to that in Example 1. The reaction results are shown in Table 1.

Embodiment 2

[0035] The difference between the catalyst preparation process of Example 2 and Example 1 is that 1 g of hydrated ruthenium trichloride is dissolved in 100 ml of methanol to finally obtain a nitrogen-doped carbon-supported ruthenium catalyst (Ru@N-C).

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Abstract

The application discloses a method for preparing anisaldehyde by catalytic liquid-phase selective oxidation. In this method, the material containing fluorinated alcohol compounds and p-methoxytoluene is contacted with a catalyst in the presence of an oxygen source to react to obtain anisaldehyde; wherein, air or oxygen is used as an oxygen source, and Nitrogen-doped carbon-supported metals were used as catalysts, and fluorinated alcohols were used as solvents to catalyze the liquid-phase selective oxidation of p-methoxytoluene to produce anisaldehyde. The method has the advantages of mild reaction conditions, high raw material conversion rate and product selectivity, recyclable catalyst, etc. The conversion rate of p-methoxytoluene can reach more than 70%, and the selectivity of anisaldehyde can reach more than 90%.

Description

technical field [0001] The application relates to a method for preparing anisaldehyde by selective oxidation of chemical liquid phase, and belongs to the technical field of organic chemical industry. Background technique [0002] Anisaldehyde, also known as p-methoxybenzaldehyde, is an edible spice permitted by the "National Food Safety Standard for the Use of Food Additives" (GB2760-2014), mainly used for the preparation of vanilla, spices, apricot, cream, fennel, caramel , cherry, chocolate, walnut, raspberry, strawberry, mint and other flavors. It is also used as a color developer, a brightener for environmental-friendly cyanide-free zinc plating DE additives, and an intermediate for the synthesis of amoxicillin. [0003] The traditional preparation method of anisaldehyde has the following problems: (1) Anethole (p-propenyl anisole) oxidation method. The raw material of the method is a natural product, the source is limited, and the cost is high. (2) Phenol reacts with...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C45/36C07C47/575B01J27/24
CPCC07C45/36B01J27/24C07C47/575Y02P20/584
Inventor 黄义争高进徐杰孙颖郑玺苗虹马红马继平
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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