Synthetic process for p-methoxy benzaldehyde

A technology of p-methoxybenzaldehyde and p-methoxytoluene, which is applied in the field of synthesis of p-methoxybenzaldehyde, can solve problems such as environmental pollution, achieve the effect of easy separation and recovery, and avoid pollution

Inactive Publication Date: 2004-04-28
大化集团有限责任公司研究院 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the early days, the preparation of p-methoxybenzaldehyde mostly used stoichiometric oxidation methods, such as using Mn2O5 as the oxidizing agent or chlorination method. The preparation process of this method often produced a large number of by-products, which caused great pollution to the environment.

Method used

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  • Synthetic process for p-methoxy benzaldehyde

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] 1) Preparation of CoO-Al 2 o 3 catalyst

[0015] Dissolve 20 grams of cobalt nitrate in 100 ml of denatured alcohol, then add 30 grams of Al with a size of 15-60 nanometers 2 o 3 , soaked for 24 hours, filtered and roasted at 450°C for 4 hours to obtain the main catalyst;

[0016] 2) to buy technical grade benzoyl peroxide or azobisisobutyrocyanide as co-catalyst; present embodiment adopts benzoyl peroxide;

[0017] 3) Add 100 grams of acetic acid solvent, 30 grams of p-methoxytoluene, 0.3 grams of main catalyst, and 0.02 grams of benzoyl peroxide into an autoclave with a volume of 250 ml respectively, heat up to 100° C. under stirring, and then use oxygen Stamping to 0.6Mpa, after constant temperature reaction for 1 hour, the temperature is lowered, and the reaction stops.

[0018] GLC sampling analysis: acetic acid (80 g) was distilled off under normal pressure, and the recovery rate was 80%. P-methoxytoluene (15g) and 120 aldehydes (20g) were evaporated under r...

Embodiment 2

[0021] The difference from Example 1 is:

[0022] Preparation of CoO-Al 2 o 3 catalyst

[0023] Dissolve 20 grams of cobalt nitrate in 100 ml of denatured alcohol, then add 30 grams of Al with a size of 15-60 nanometers 2 o 3 , soaked for 36 hours, filtered and roasted at 500°C for 4 hours to obtain the main catalyst;

[0024] Add 100 grams of acetic acid, 30 grams of p-methoxytoluene, 0.1 grams of main catalyst, and 0.02 grams of azobisisobutyrocyanide into a 250ml autoclave, heat up to 100°C under stirring, and then press it to 1.0 with oxygen Mpa, after 2 hours of constant temperature reaction, the temperature was lowered, and the reaction stopped.

[0025] GLC sampling analysis: acetic acid (80 g) was distilled off under normal pressure, and the recovery rate was 80%. P-methoxytoluene (16g) and 120 aldehydes (18g) were distilled off under reduced pressure, the yield was 60%, and the total yield of p-methoxybenzaldehyde reached 86%.

Embodiment 3

[0027] The difference from Example 1 is:

[0028] Preparation of CoO-Al 2 o 3 catalyst

[0029] Dissolve 20 grams of cobalt nitrate in 200 ml of industrial alcohol, then add 80 grams of Al with a size of 15-60 nanometers 2 o 3 , soaked for 48 hours, filtered and roasted at 500°C for 4 hours to obtain the main catalyst;

[0030] Add 100 grams of acetic acid, 30 grams of p-methoxytoluene, 0.3 grams of main catalyst, and 0.015 grams of benzoyl peroxide into a 250ml autoclave, heat up to 135°C while stirring, and then press it to 1.2Mpa with oxygen , After constant temperature reaction for 1 hour, the temperature was lowered to stop the reaction.

[0031] GLC sampling analysis: acetic acid (80 g) was distilled off under normal pressure, and the recovery rate was 80%. P-methoxytoluene (15g) and 120 aldehydes (19g) were distilled off under reduced pressure, with a yield of 63.3%, and the total yield of p-methoxybenzaldehyde reached 85%.

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Abstract

The present invention relates to methoxy benzaldehyde compound, and is especially a catalytic oxidation process of synthesizing p-methoxy benzaldehyde. Methoxy methylbenzene material is oxidized with oxygen as oxygen source under the action of the catalyst CoO-Al2O3-R to synthesize p-methoxy benzaldehyde. In the catalytic oxidation process, nano level catalyst is dispersed in the reaction system homogeneously and may be recovered easily. The catalyst has p-methoxy benzaldehyde selectivity up to 92 %, and the catalytic oxidation process has single-path yield of 66 % and total yield up to 90 % and no environmental pollution, and is one clean and efficient technological process.

Description

technical field [0001] The present invention relates to methoxybenzaldehyde compound, specifically a kind of synthetic method of p-methoxybenzaldehyde. Background technique [0002] Methoxybenzaldehyde is an important intermediate in the synthesis of fragrances, medicines, and pesticides, also known as anisaldehyde. In the early days, the preparation of p-methoxybenzaldehyde mostly used stoichiometric oxidation methods, such as using Mn2O5 as the oxidizing agent or the method of chlorination. The preparation process of this method often produced a large number of by-products, which caused great pollution to the environment. Contents of the invention [0003] The purpose of the present invention is to provide a kind of synthetic method that is easy to reclaim, the p-methoxybenzaldehyde of environmental protection. [0004] In order to achieve the above object, technical scheme of the present invention is: [0005] With p-methoxytoluene as raw material and oxygen as oxygen...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/28C07C47/575
Inventor 高绪国王作旭李秋江阎圣刚
Owner 大化集团有限责任公司研究院
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